ChemicalBook CAS DataBase List 2,5-DICHLOROBENZYLAMINE

2,5-DICHLOROBENZYLAMINE synthesis

3synthesis methods

Product Name:2,5-DICHLOROBENZYLAMINE
CAS Number:10224-70-1
Molecular formula:C7H7Cl2N
Molecular Weight:176.04

Acetamide, N-(2,5-dichlorophenyl)-N-methyl-

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Yield:-

Reaction Conditions:

Stage #1: acetic acid-(2,5-dichloro-N-methyl-anilide)with borane-THF in tetrahydrofuran at 20; for 2 h;
Stage #2: with citric acid in tetrahydrofuran;water;

Steps:

16.1

To formic acid (87 eq.) was added dropwise acetic anhydride (19 eq.). After 10 minutes at O⁰C the mixture was stirred for 1 hour at room temperature. To the mixture was then added dropwise 2,5-dichloroaniline. After 1 hour the solvents were removed under vacuum and the residue was left under high vacuum for 3 hours. The solid obtained was suspended in dry THF at 0⁰C, borane IM in THF (3.0 eq.) was added slowly and the mixture was stirred, for 2 hours at room temperature. The reaction was quenched with a solution 10% of citric acid. THF was evaporated and EtOAc was added. The organic EPO phase was separated and dried over Na2SO4, filtered and concentrated to dryness under vacuum. The title compound was obtained as a white solid. MS m/z: 176 (M+H)⁺.

References:

WO2006/37468,2006,A1 Location in patent:Page/Page column 47-48

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References

95-82-9 Synthesis

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References

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