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ChemicalBook CAS DataBase List tert-Butyl 2-methylcarbazate
21075-83-2

tert-Butyl 2-methylcarbazate synthesis

10synthesis methods
-

Yield:21075-83-2 82%

Reaction Conditions:

with sodium hydrogencarbonate in tetrahydrofuran;water; pH=10 at 5; for 12 h;

Steps:

1 Reference Example 1 Preparation of 1-boc-1-methylhydrazine (Compound of Formula I)
7.2 g of methylhydrazine sulphate (49.9 mmol) was added to 144 ml of water, cooled to 5 ° C, 4.6 g of NaHCO 3 solid was added, and the pH was adjusted to 10 with aqueous NaOH.A solution of 144 ml (Boc) 2 O (49.95 mmol) in tetrahydrofuran was added dropwise, and the mixture was stirred for 12 h, and the reaction was completely observed by TLC (developing solvent: petroleum ether / ethyl acetate = 2 / 1).Extracted with ethyl acetate (100 ml × 3), and the organic phase was combined and washed with brine.Dry over anhydrous sodium sulfate and concentrate under reduced pressure.6.0 g (yield 82%) of a colorless transparent liquid compound of formula I was obtained.

References:

Shanghai Pharmaceutical Industry Institute;Zhengda Tianqing Pharmaceutical Group Co., Ltd.;Wang Huanyu;Liu Xiangkui;Yu Jingping;Zhu Xueyan;Cheng Xingdong;Zhang Aiming;Zhang Xiquan CN108129357, 2018, A Location in patent:Paragraph 0102; 0104

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