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

HRID 35522ノート

反応式

HRID 35522 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ba378ed7f98445bb9efca829e2937753
出典データセット
uspto-grants-1988_08
特許番号
US04767756

反応ノート

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