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

HRID 1681094

反応式

HRID 1681094 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

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.

後処理

  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))

出典と根拠

ORDレコード
ord-c17f1f7a1c5344879a1e59beccd67870
出典データセット
uspto-grants-1992_12
特許番号
US05169428

関連ノート

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