3,4,5,6-Tetrahydrophthalic anhydride → N-(4-chloro-5-hydroxymethylphenyl)-3,4,5,6-tetrahydrophthalimide

HRID 1681094

반응식

HRID 1681094 반응식
[C:1]1(=[O:11])[O:6][C:4](=O)[C:3]2[CH2:7][CH2:8][CH2:9][CH2:10][C:2]1=2.[Cl:12][C:13]1[C:19]([CH2:20][OH:21])=[CH:18][C:16]([NH2:17])=[CH:15][CH:14]=1>C(O)(=O)C>[Cl:12][C:13]1[C:19]([CH2:20][OH:21])=[CH:18][C:16]([N:17]2[C:1](=[O:11])[C:2]3[CH2:10][CH2:9][CH2:8][CH2:7][C:3]=3[C:4]2=[O:6])=[CH:15][CH:14]=1

참가 물질

4

반응물 2

HCID 124753,4,5,6-Tetrahydrophthalic anhydrideHCID 13567962(5-Amino-2-chlorophenyl)methanol

생성물 1

HCID 14277448N-(4-chloro-5-hydroxymethylphenyl)-3,4,5,6-tetrahydrophthalimide수율 38.4%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

To 50 ml of acetic acid, 2.47 g of 3,4,5,6-tetrahydrophthalic anhydride and2.56 g of 4-chloro-5-hydroxymethyl aniline were added and the mixture was heated to reflux under stirring for 16 hours. After cooling, the solvent was evaporated under reduced pressure and the residue was purified by column chromatography (silica gel, benzene/ethyl acetate=10/1 (v/v)) to obtain 1.82 g of the desired product.

후처리

  1. temperaturethe mixture was heated
  2. temperatureto reflux
  3. temperatureAfter cooling
  4. customthe solvent was evaporated under reduced pressure
  5. customthe residue was purified by column chromatography (silica gel, benzene/ethyl acetate=10/1 (v/v))

출처 및 근거

ORD 기록
ord-c17f1f7a1c5344879a1e59beccd67870
출처 데이터셋
uspto-grants-1992_12
특허 번호
US05169428

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