Methyl 7-chloro-2-methyl-[1,2,4]triazolo[1,5-a]pyrimidine-5-carboxylate → HCID 178498634, 화합물

HRID 1755882노트

반응식

HRID 1755882 반응식
Cl[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][CH3:15])=[O:13])[CH:3]=1.O.[SH2:17].[Na]>CO>[SH:17][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][CH3:15])=[O:13])[CH:3]=1

참가 물질

4

반응물 2

HCID 14852618Methyl 7-chloro-2-methyl-[1,2,4]triazolo[1,5-a]pyrimidine-5-carboxylateHCID 53442613Sodium hydrogen sulfide hydrate

생성물 1

HCID 178498634HCID 178498634, 화합물수율 83.4%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
60 °C

실험 절차

Methyl 7-chloro-2-methyl-s-triazolo[1,5-a]pyrimidine-5-carboxylate (0.80 g) (3.53 mmol) are suspended in 35 ml of methanol and treated with 0.78 g (10.6 mmol) of sodium hydrogen sulphide hydrate. After stirring at 60° C. for 5 hours the mixture is concentrated and the residue is dissolved in 20 ml of water. The solution is acidified to pH 3 with 3N aqueous hydrochloric acid. The separated product is filtered off under suction and washed with water and methanol. After recrystallization from methanol/dichloromethane there is obtained 0.66 g of methyl 7-mercapto-2-methyl-s-triazolo[1,5-a]pyrimidine-5-carboxylate as yellow crystals of melting point 237° C. (dec.).

후처리

  1. concentrationis concentrated
  2. dissolutionthe residue is dissolved in 20 ml of water
  3. filtrationThe separated product is filtered off under suction
  4. washwashed with water and methanol
  5. customAfter recrystallization from methanol/dichloromethane there

출처 및 근거

ORD 기록
ord-b36d5428d7ec4ddba2d7a016e7914e75
출처 데이터셋
uspto-grants-1995_08
특허 번호
US05438052

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