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Hydrochloric Acid → HCID 11058732、化合物

HRID 1870259
ノート
印刷プレビュー

反応式

HRID 1870259 の反応式
C[C@@H]([O:8][C:9]([CH2:11][C@@H:12]1[C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=2[N:16]([C:23](=[O:36])[C:24]2[CH:29]=[CH:28][C:27]([N:30]3[CH2:34][CH2:33][CH2:32][CH2:31]3)=[CH:26][C:25]=2[Cl:35])[CH2:15][CH2:14][CH2:13]1)=[O:10])CCCCC.[OH-].[Na+].Cl>CO>[C:9]([CH2:11][C@@H:12]1[C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=2[N:16]([C:23](=[O:36])[C:24]2[CH:29]=[CH:28][C:27]([N:30]3[CH2:31][CH2:32][CH2:33][CH2:34]3)=[CH:26][C:25]=2[Cl:35])[CH2:15][CH2:14][CH2:13]1)([OH:10])=[O:8]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium Hydroxide2 回HCID 10973260HCID 10973260、化合物

生成物 1

HCID 11058732HCID 11058732、化合物収率 79.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
45 °C

実験手順

To a suspension of (5R)-5-((R)-2-heptyloxycarbonylmethyl)-1-[4-(1-pyrrolidinyl)-2-chlorobenzoyl]-2,3,4,5-tetrahydro-1H-benzazepine (33 g) in methanol (500 ml) is added a 5N aqueous sodium hydroxide solution (25.8 ml), and the mixture is heated with stirring at 40-50° C. for two hours. To the mixture is further added a 5N aqueous sodium hydroxide solution (15 ml), and the mixture is heated with stirring at 50° C. for three hours. The reaction solution is acidified with hydrochloric acid, and concentrated under reduced pressure to remove the methanol, and extracted with ethyl acetate. The ethyl acetate layer is washed with water, dried over magnesium sulfate, and concentrated under reduced pressure to remove the ethyl acetate. The resultant is crystallized from ethyl acetate--diethyl ether, washed with diethyl ether--n-hexane to give (5R)-5-carboxymethyl-1-[4-(1-pyrrolidinyl)-2-chlorobenzoyl]-2,3,4,5-tetrahydro-1H-benzazepine (21.1 g).

後処理

  1. temperaturethe mixture is heated
  2. temperaturethe mixture is heated
  3. stirringwith stirring at 50° C. for three hours
  4. concentrationconcentrated under reduced pressure
  5. customto remove the methanol
  6. extractionextracted with ethyl acetate
  7. washThe ethyl acetate layer is washed with water
  8. dry with materialdried over magnesium sulfate
  9. concentrationconcentrated under reduced pressure
  10. customto remove the ethyl acetate
  11. customThe resultant is crystallized from ethyl acetate
  12. washdiethyl ether, washed with diethyl ether

出典と根拠

ORDレコード
ord-290e5f27099b44e2b7aa60126adeee46
出典データセット
uspto-grants-2000_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06096736

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート