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Sodium Hydroxide → N-(2-hydroxy-4-methoxybenzoyl)cysteamine

HRID 465917
ノート
印刷プレビュー

反応式

HRID 465917 の反応式
C(OC([O:6][C:7]1[CH:18]=[C:17]([O:19][CH3:20])[CH:16]=[CH:15][C:8]=1[C:9]([NH:11][CH2:12][CH2:13][SH:14])=[O:10])=O)C.[OH-].[Na+]>CO>[OH:6][C:7]1[CH:18]=[C:17]([O:19][CH3:20])[CH:16]=[CH:15][C:8]=1[C:9]([NH:11][CH2:12][CH2:13][SH:14])=[O:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 14719509N-(2-ethoxycarbonyloxy-4-methoxybenzoyl)cysteamine

生成物 1

HCID 14719510N-(2-hydroxy-4-methoxybenzoyl)cysteamine収率 77%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

4.50 g of the N-(2-ethoxycarbonyloxy-4-methoxybenzoyl)cysteamine was dissolved in 70 ml of methanol, and 17 ml of 2N aqueous solution of sodium hydroxide was added to the solution. The mixture was agitated for 45 minutes. The solvent was distilled off in evacuated atomosphere, and 2N aqueous solution of sodium hydroxide and methylene chloride were added to the mixture for separation. The aqueous phase was further washed with methylene chloride, acidified by adding 6N aqueous hydrochloric acid, and extracted with methylene chloride. The mixture was dried over anhydrous sodium sulfate, and the solvent was distilled off in evacuated atomosphere. The residue was subjected to column chromatography using silica gel, and there was obtained 2.63 g of N-(2-hydroxy-4-methoxybenzoyl)cysteamine (I).

後処理

  1. distillationThe solvent was distilled off in evacuated atomosphere, and 2N aqueous solution of sodium hydroxide and methylene chloride
  2. additionwere added to the mixture for separation
  3. washThe aqueous phase was further washed with methylene chloride
  4. additionby adding 6N aqueous hydrochloric acid
  5. extractionextracted with methylene chloride
  6. dry with materialThe mixture was dried over anhydrous sodium sulfate
  7. distillationthe solvent was distilled off in evacuated atomosphere

出典と根拠

ORDレコード
ord-5a046f7703cc45c78a8c2b05cba0d8dc
出典データセット
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05155106

反応ノート

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