Water → 3-Carbomethoxy-4-[(chloroacetyl)amino]thiophene

HRID 67431

반응식

HRID 67431 반응식
Cl.[C:2]([C:6]1[C:10]([NH2:11])=[CH:9][S:8][CH:7]=1)([O:4][CH3:5])=[O:3].[Cl:12][CH2:13][C:14](Cl)=[O:15].C(N(CC)CC)C.O>C(Cl)Cl>[C:2]([C:6]1[C:10]([NH:11][C:14](=[O:15])[CH2:13][Cl:12])=[CH:9][S:8][CH:7]=1)([O:4][CH3:5])=[O:3]

참가 물질

6

반응물 4

HCID 962WaterHCID 6577Chloroacetyl chlorideHCID 8471TriethylamineHCID 2777609Methyl 4-aminothiophene-3-carboxylate Hydrochloride

생성물 1

HCID 145100033-Carbomethoxy-4-[(chloroacetyl)amino]thiophene

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A suspension of 12.2 g (0.063 mol) of 3-carbomethoxy-4-aminothiophene hydrochloride in 100 ml of methylene chloride is treated with 10 ml (0.126 mol) of chloroacetyl chloride and subsequently dropwise with 17.6 ml (0.126 mol) of triethylamine, the temperature being held below 25° C. The solution is poured into water and extracted twice with 50 ml of methylene chloride each time. The combined methylene chloride extracts are washed three times with 50 ml of water each time, dried over magnesium sulphate and evaporated. After chromatography on silica gel using methylene chloride for the elution, there is obtained crystalline 3-carbomethoxy-4-[(chloroacetyl)amino]thiophene of melting point 98°-100° C.

후처리

  1. custombeing held below 25° C
  2. extractionextracted twice with 50 ml of methylene chloride each time
  3. washThe combined methylene chloride extracts are washed three times with 50 ml of water each time
  4. dry with materialdried over magnesium sulphate
  5. customevaporated
  6. washfor the elution

출처 및 근거

ORD 기록
ord-9fc64a80331f4f7b8dc44e2e238bbba8
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04346032

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