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2-(CHLOROMETHYL)-5,6,7,8-TETRAHYDRO[1]BENZOTHIENO[2,3-D]PYRIMIDIN-4-AMINE synthesis

2synthesis methods
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Yield:89567-04-4 63.4%

Reaction Conditions:

Stage #1: 3-cyano-2-amino-4,5,6,7-tetrahydrobenzo[b]thiophene;chloroacetonitrile in 1,4-dioxane at 80; for 0.166667 h;
Stage #2: with hydrogenchloride in 1,4-dioxane;water; for 6 h;

Steps:

1.2

(2) 1.0 g of 2-amino-3-nitrile-4,5,6,7-tetrahydrobenzothiophene and 1 ml of chloroacetonitrile,With 15ml dioxane dissolved in the reaction flask, 80 ° C for 10min after the addition of hydrochloric acid 20ml, the reaction 6h, the reaction mixture was cooled and poured into ice water,Add ammonia to slightly alkaline, a large number of solid precipitation, filtration with petroleum ether: ethyl acetate 3: 1The eluent was passed through the column to give 0.9 g of 2-chloromethyl-4-amino-5,6,7,8-tetrahydrobenzothieno [2,3-d] pyrimidine in a yield of 63.4%.

References:

CN104945412,2018,B Location in patent:Paragraph 0043; 0046