Hydrochloric Acid → 7-Chloro-1,3,4,5-tetrahydro-3-(methoxycarbonyl)-4-(4-methoxyphenyl)-2H-1-benzazepin-2-one

HRID 35522노트

반응식

HRID 35522 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1[CH2:9][CH:10]([CH:19]([C:24]([O:26][CH3:27])=[O:25])[C:20](OC)=[O:21])[C:11]1[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[CH:13][CH:12]=1.C[O-].[Na+].Cl>CO>[Cl:8][C:5]1[CH:6]=[CH:7][C:2]2[NH:1][C:20](=[O:21])[CH:19]([C:24]([O:26][CH3:27])=[O:25])[CH:10]([C:11]3[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[CH:13][CH:12]=3)[CH2:9][C:3]=2[CH:4]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 10942334Sodium MethoxideHCID 14156189[2-(2-Amino-5-chlorophenyl)-1-(4-methoxyphenyl)ethyl]propanedioic acid, dimethyl ester

생성물 1

HCID 141561947-Chloro-1,3,4,5-tetrahydro-3-(methoxycarbonyl)-4-(4-methoxyphenyl)-2H-1-benzazepin-2-one수율 91.5%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

To a solution of [2-(2-amino-5-chlorophenyl)-1-(4-methoxyphenyl)ethyl]propanedioic acid, dimethyl ester (23.2 g, 59.2 mmole) in methanol (200 ml) was added a 25% solution of sodium methoxide in methanol (16 ml, 69.97 mmole). The solution was refluxed for 3 hours under argon. The reaction was cooled to room temperature and treated with 200 ml of 1N hydrochloric acid. The white precipitate was filtered and washed with water, methanol, and dried in vacuo to yield 19.5 g of the title compound, melting point 189°-190.5° C.

후처리

  1. temperatureThe solution was refluxed for 3 hours under argon
  2. filtrationThe white precipitate was filtered
  3. washwashed with water, methanol
  4. customdried in vacuo

출처 및 근거

ORD 기록
ord-ba378ed7f98445bb9efca829e2937753
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04767756

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