Chlorosuccinimide → Methyl 5-chloro-4-(4-chloro-1-ethyl-1H-pyrazol-5-yl)-2-thiophenecarboxylate

HRID 1961280노트

반응식

HRID 1961280 반응식
[Cl:1][C:2]1[S:6][C:5]([C:7]([O:9][CH3:10])=[O:8])=[CH:4][C:3]=1/[C:11](/[N:14]([CH2:17][CH3:18])[N:15]=[CH2:16])=[CH:12]/C.[Cl:19]N1C(=O)CCC1=O>C1COCC1>[Cl:1][C:2]1[S:6][C:5]([C:7]([O:9][CH3:10])=[O:8])=[CH:4][C:3]=1[C:11]1[N:14]([CH2:17][CH3:18])[N:15]=[CH:16][C:12]=1[Cl:19]

참가 물질

4

반응물 2

HCID 31398ChlorosuccinimideHCID 68670418Methyl 5-chloro-4-[(1Z)-1-(1-ethyl-2-methylidenehydrazino)-1-propen-1-yl]-2-thiophenecarboxylate

생성물 1

HCID 57826495Methyl 5-chloro-4-(4-chloro-1-ethyl-1H-pyrazol-5-yl)-2-thiophenecarboxylate수율 95.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Methyl 5-chloro-4-[(1Z)-1-(1-ethyl-2-methylidenehydrazino)-1-propen-1-yl]-2-thiophenecarboxylate (260 mg, 0.96 mmol) and 1-chloro-2,5-pyrrolidinedione (154 mg, 1.15 mmol) in THF (4 mL) were heated at 70° C. under N2 for 2 h, concentrated and purified on silica (EtOAc/Hex, 10-30%) to afford the title compound (0.281 g, 83%) as a syrup: LC-MS (ES) m/z=305 (M+H)+.

후처리

  1. concentrationconcentrated
  2. custompurified on silica (EtOAc/Hex, 10-30%)

출처 및 근거

ORD 기록
ord-a237d9e9097442748de23216991eb323
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08410158B2

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