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Acetic Anhydride → HCID 178488951, 화합물

HRID 235960
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HRID 235960 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 7918Acetic AnhydrideHCID 135671327HCID 135671327, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 178488951HCID 178488951, 화합물수율 84%

시약·촉매·용매 2

HCID 23939Platinum촉매HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-94915cc999144073835cdb7647951dec
출처 데이터셋
uspto-grants-1987_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04642311

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