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Acetic Anhydride → HCID 178488951、化合物

HRID 235960
ノート
印刷プレビュー

反応式

HRID 235960 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[NH:10][C:11]([N+:15]([O-])=O)=[C:12]([CH3:14])[N:13]=2)=[CH:5][CH:4]=1.[C:18](OC(=O)C)(=[O:20])[CH3:19].[H][H]>CC(O)=O.[Pt]>[C:18]([NH:15][C:11]1[NH:10][C:9]([C:6]2[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)=[N:13][C:12]=1[CH3:14])(=[O:20])[CH3:19]
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 3

HCID 7918Acetic AnhydrideHCID 135671327HCID 135671327、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 178488951HCID 178488951、化合物収率 84%

試薬・触媒・溶媒 2

HCID 23939Platinum触媒HCID 176Acetic Acid溶媒

実験手順

A solution of 41 (3.5 g, 0.015 mole) dissolved in glacial HOAc (35 ml)--acetic anhydride (105 ml) was hydrogenated at 50 psi over 5% platinum on charcoal catalyst (0.75 g) until uptake of hydrogen was complete. Catalyst was filtered off and the filtrate was evaporated to dryness under reduced pressure. The residue was dissolved in H2O (50 ml) and heated on a steam bath for 1 hour. The cooled solution was washed with ether (4×10 ml) and then evaporated to dryness in vacuo. Recrystallization of the residue from CHCl3 gave 3.07 g (84%) of 42 in two crops; m.p. 202°-204° C.

後処理

  1. filtrationCatalyst was filtered off
  2. customthe filtrate was evaporated to dryness under reduced pressure
  3. dissolutionThe residue was dissolved in H2O (50 ml)
  4. temperatureheated on a steam bath for 1 hour
  5. washThe cooled solution was washed with ether (4×10 ml)
  6. customevaporated to dryness in vacuo
  7. customRecrystallization of the residue from CHCl3

出典と根拠

ORDレコード
ord-94915cc999144073835cdb7647951dec
出典データセット
uspto-grants-1987_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04642311

反応ノート

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