5-Chloro-2-methoxybenzoyl chloride → 2-Ethoxy-4-(5-chloro-2-methoxy-benzamido)-benzoic acid ethyl ester

HRID 27467노트

반응식

HRID 27467 반응식
[CH2:1]([O:3][C:4](=[O:15])[C:5]1[CH:10]=[CH:9][C:8]([NH2:11])=[CH:7][C:6]=1[O:12][CH2:13][CH3:14])[CH3:2].[Cl:16][C:17]1[CH:18]=[CH:19][C:20]([O:26][CH3:27])=[C:21]([CH:25]=1)[C:22](Cl)=[O:23]>C(N(CC)CC)C.C1(C)C=CC=CC=1>[CH2:1]([O:3][C:4](=[O:15])[C:5]1[CH:10]=[CH:9][C:8]([NH:11][C:22](=[O:23])[C:21]2[CH:25]=[C:17]([Cl:16])[CH:18]=[CH:19][C:20]=2[O:26][CH3:27])=[CH:7][C:6]=1[O:12][CH2:13][CH3:14])[CH3:2]

참가 물질

5

반응물 2

HCID 123841765-Chloro-2-methoxybenzoyl chlorideHCID 54179514Benzoic acid, 4-amino-2-ethoxy-, ethyl ester

생성물 1

HCID 538402982-Ethoxy-4-(5-chloro-2-methoxy-benzamido)-benzoic acid ethyl ester

시약·촉매·용매 2

HCID 1140Toluene용매2회HCID 8471Triethylamine용매

실험 절차

10.4 g of 2-ethoxy-4-amino-benzoic acid ethyl ester were suspended in a mixture of 6.8 ml of triethylamine and 200 ml of toluene and 10.3 g of 5-chloro-2-methoxy-benzoyl chloride dissolved in a small amount of toluene were added dropwise. The whole was stirred for 3 hours under reflux and, after cooling, it was washed with water, dilute hydrochloric acid and a sodium bicarbonate solution and dried over sodium sulfate. Upon concentration of the solution under reduced pressure, the 2-ethoxy-4-(5-chloro-2-methoxy-benzamido)-benzoic acid ethyl ester was obtained in the form of a solid product having a crude melting point of 108°-111° C.

후처리

  1. additionwere added dropwise
  2. temperatureunder reflux
  3. temperatureafter cooling
  4. washit was washed with water, dilute hydrochloric acid
  5. dry with materiala sodium bicarbonate solution and dried over sodium sulfate

출처 및 근거

ORD 기록
ord-72bd60edce5b4c00965ff9f142800b3b
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04221815

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