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Sodium Hydroxide → 2-[(3,4-Dichloro-6,7,8,8a,9,10-hexahydro-6-oxo-8a-propyl-2-phenanthrenyl)oxy]ethanimidamide hydrochloride

HRID 867992
ノート
印刷プレビュー

反応式

HRID 867992 の反応式
[Cl:1][C:2]1[C:3]([O:21][CH2:22][C:23]#[N:24])=[CH:4][C:5]2[CH2:6][CH2:7][C:8]3([CH2:18][CH2:19][CH3:20])[C:13]([C:14]=2[C:15]=1[Cl:16])=[CH:12][C:11](=[O:17])[CH2:10][CH2:9]3.C[O-].[Na+].[Cl-].[NH4+:29].[OH-].[Na+]>CO>[ClH:1].[Cl:1][C:2]1[C:3]([O:21][CH2:22][C:23](=[NH:29])[NH2:24])=[CH:4][C:5]2[CH2:6][CH2:7][C:8]3([CH2:18][CH2:19][CH3:20])[C:13]([C:14]=2[C:15]=1[Cl:16])=[CH:12][C:11](=[O:17])[CH2:10][CH2:9]3
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 14798Sodium HydroxideHCID 25517Ammonium ChlorideHCID 10942334Sodium MethoxideHCID 212895702-[(3,4-Dichloro-6,7,8,8a,9,10-hexahydro-6-oxo-8a-propyl-2-phenanthrenyl)oxy]acetonitrile

生成物 1

HCID 212895732-[(3,4-Dichloro-6,7,8,8a,9,10-hexahydro-6-oxo-8a-propyl-2-phenanthrenyl)oxy]ethanimidamide hydrochloride

試薬・触媒・溶媒 1

HCID 887
Methanol
溶媒

実験手順

To a solution of 2-[(3,4-Dichloro-6,7,8,8a,9,10-hexahydro-6-oxo-8a-propyl-2-phenanthrenyl)oxy]acetonitrile (200 mg, 0.549 mmole) in methanol (3 ml ) is added sodium methoxide (10 mg). After stirring for 1 hour ammonium chloride (53.5 mg, 1 mmole) is added and stirring is continued for 2 hours. The reaction mixture is poured into ice water containing 0.5 ml of 10N sodium hydroxide extracted with ether, washed with water dried over potassium carbonate, filtered and acidified with 10N ethanolic hydrochloric acid to precipitate 2-[(3,4-Dichloro-6,7,8,8a,8,10-hexahydro-6-oxo-8a-propyl-2-phenanthrenyl)oxy]ethanimidamide hydrochloride.

後処理

  1. additionis added
  2. extractionextracted with ether
  3. washwashed with water
  4. dry with materialdried over potassium carbonate
  5. filtrationfiltered
  6. customto precipitate 2-[(3,4-Dichloro-6,7,8,8a,8,10-hexahydro-6-oxo-8a-propyl-2-phenanthrenyl)oxy]ethanimidamide hydrochloride

出典と根拠

ORDレコード
ord-e37525cf3aea493084107c30d30c4048
出典データセット
uspto-grants-1988_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04777281

反応ノート

読み込み中…

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