Hydrochloric Acid → HCID 178432397, 화합물

HRID 1755883노트

반응식

HRID 1755883 반응식
[SH:1][C:2]1[N:7]2[N:8]=[C:9]([CH3:11])[N:10]=[C:6]2[N:5]=[C:4]([C:12]([O:14]C)=O)[CH:3]=1.[NH2:16][OH:17].Cl>CO>[OH:17][NH:16][C:12]([C:4]1[CH:3]=[C:2]([SH:1])[N:7]2[N:8]=[C:9]([CH3:11])[N:10]=[C:6]2[N:5]=1)=[O:14]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 787HydroxylamineHCID 178498634HCID 178498634, 화합물

생성물 1

HCID 178432397HCID 178432397, 화합물수율 107.5%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Methyl 7-mercapto-2-methyl-s-triazolo[1,5-a]pyrimidine-5-carboxylate (500 mg) (2.23 mmol) are suspended in 100 ml of absolute methanol. 2.95 mg (8.9 mmol) of hydroxylamine are added within 4 days while stirring. The reaction mixture is acidified (pH 6) with 3N aqueous hydrochloric acid. The product is filtered off under suction and washed in succession with water, methanol and diethyl ether. There are obtained 540 mg of N-hydroxy-7-mercapto-2-methyl-s-triazolo[1,5-a]pyrimidine-5-carboxamide as yellow crystals of melting point 178°-179° C.

후처리

  1. filtrationThe product is filtered off under suction
  2. washwashed in succession with water, methanol and diethyl ether

출처 및 근거

ORD 기록
ord-86b72fd49362429bb0d7ecf901dbddb4
출처 데이터셋
uspto-grants-1995_08
특허 번호
US05438052

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