Methanol → HCID 22414561, 화합물

HRID 1721314노트

반응식

HRID 1721314 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[S:10])[NH2:9])=[CH:4][C:3]=1[CH3:11].NOS(O)(=O)=O.CO.[N:20]1C=CC=[CH:22][CH:21]=1>COC(OC)(N(C)C)C.ClCCl>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[S:10][N:20]=[C:21]([CH3:22])[N:9]=2)=[CH:4][C:3]=1[CH3:11]

참가 물질

7

반응물 4

HCID 887MethanolHCID 1049PyridineHCID 76284hydroxylamine-O-sulfonic acidHCID 21833829Benzenecarbothioamide, 4-bromo-3-methyl-

생성물 1

HCID 22414561HCID 22414561, 화합물

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 878351,1-Dimethoxyethyl(dimethyl)amine용매

실험 절차

A solution of 4-bromo-3-methylbenzenecarbothioamide (1.20 g) in dimethylacetamide dimethyl acetal (2 ml) and dichloromethane (30 ml) was stirred under nitrogen at room temperature for 7 h. The solvent was evaporated in vacuo to give a dark brown oil to which was added hydroxylamine-O-sulphonic acid (0.88 g), methanol (20 ml) and pyridine (0.83 ml) and the mixture stirred at room temperature under nitrogen for 16 h. After evaporation, aqueous potassium carbonate was added and the mixture was extracted with dichloromethane. The combined extracts were dried and evaporated to give a brown residue which was purified by column chromatography on silica eluting with hexane:ethyl acetate (4:1) to give the title compound as an orange solid (0.8 g). T.l.c.hexane:ethyl acetate (4:1), Rf=0.52

후처리

  1. customThe solvent was evaporated in vacuo
  2. customto give a dark brown oil to which
  3. customAfter evaporation, aqueous potassium carbonate
  4. additionwas added
  5. extractionthe mixture was extracted with dichloromethane
  6. customThe combined extracts were dried
  7. customevaporated
  8. customto give a brown residue which
  9. customwas purified by column chromatography on silica eluting with hexane:ethyl acetate (4:1)

출처 및 근거

ORD 기록
ord-3273824991e94518be246d9bae1b3b69
출처 데이터셋
uspto-grants-1996_04
특허 번호
US05510350

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