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HCID 15098931, 화합물 → HCID 178482028, 화합물

HRID 2290234
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HRID 2290234 반응식
[CH3:1][N:2]1[C:6]([S:7][CH2:8][CH2:9][CH2:10][C:11](Cl)=[O:12])=[N:5][N:4]=[N:3]1.N1C=CC=CC=1.[SH2:20]>C(Cl)Cl.C(Cl)(Cl)Cl>[CH3:1][N:2]1[C:6]([S:7][CH2:8][CH2:9][CH2:10][C:11]([OH:12])=[S:20])=[N:5][N:4]=[N:3]1
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참가 물질

5

반응물 2

HCID 15098931HCID 15098931, 화합물HCID 18424405HCID 18424405, 화합물

생성물 1

HCID 178482028HCID 178482028, 화합물

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 6344Dichloromethane용매2회

실험 절차

920 mg of 4-(1-methyltetrazol-5-ylthio)-butyric acid chloride are dissoved in 1.4 ml of absolute methylene chloride and added dropwise at 0° to 5.54 ml of a pyridine/H2S solution in methylene chloride (30 ml of absolute pyridine and 6 g of H2S in 100 ml of methylene chloride). The whole is then stirred for one hour at 0° under a nitrogen atmosphere. The reaction mixture is taken up in chloroform, the aqueous phase is acidified to a pH of 2 using 2N H2SO4 and extraction is carried out twice with chloroform. The combined organic phases are washed twice with 5 ml of 10% NaHCO3 solution. The pH is then adjusted to 3 using 2N H2SO4 and the title compound is extracted several times with chloroform. The title compound is obtained after drying over sodium sulphate and concentrating.

후처리

  1. extraction2N H2SO4 and extraction
  2. washThe combined organic phases are washed twice with 5 ml of 10% NaHCO3 solution
  3. extractionthe title compound is extracted several times with chloroform

출처 및 근거

ORD 기록
ord-44bcabe2256946aaaa08fe368ad638d9
출처 데이터셋
uspto-grants-1986_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04616007

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