Triethylamine → N'-(cyclopropanecarbonyl)-3-iodo-4-methylbenzohydrazide

HRID 1619147

반응식

HRID 1619147 반응식
[CH:1]1([C:4](Cl)=[O:5])[CH2:3][CH2:2]1.[I:7][C:8]1[CH:9]=[C:10]([CH:15]=[CH:16][C:17]=1[CH3:18])[C:11]([NH:13][NH2:14])=[O:12].C(N(CC)CC)C>ClCCl>[CH:1]1([C:4]([NH:14][NH:13][C:11](=[O:12])[C:10]2[CH:15]=[CH:16][C:17]([CH3:18])=[C:8]([I:7])[CH:9]=2)=[O:5])[CH2:3][CH2:2]1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 77637Cyclopropanecarbonyl chlorideHCID 597325003-Iodo-4-methylbenzohydrazide

생성물 1

HCID 965865N'-(cyclopropanecarbonyl)-3-iodo-4-methylbenzohydrazide수율 76.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of cyclopropanecarbonyl chloride (1.81 mL, 20.0 mmol) in dichloromethane (20 mL) was added dropwise to a stirred solution of 3-iodo-4-methylbenzohydrazide (preparation 55b, 5.00 g, 18.1 mmol) and triethylamine (2.78 mL, 20.0 mmol) in dichloromethane (80 mL) at 0° C. After 2 hours stirring at ambient temperature, the mixture was concentrated in vacuo and water was added to the residue. The resultant precipitate was filtered and was washed with water and diethyl ether to give the title compound (4.75 g, 76%) as a white solid.

후처리

  1. concentrationthe mixture was concentrated in vacuo and water
  2. additionwas added to the residue
  3. filtrationThe resultant precipitate was filtered
  4. washwas washed with water and diethyl ether

출처 및 근거

ORD 기록
ord-858db07679aa403c948126bf8853f46d
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08772288B2

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