Acetic Anhydride → HCID 54074224、化合物

HRID 1763169ノート

反応式

HRID 1763169 の反応式
[C:1]([O:4][C:5](=O)[CH3:6])(=O)[CH3:2].[CH2:8]([O:10][C:11]1[CH:16]=[CH:15][C:14]([C:17]([C:19]2[CH:24]=[CH:23][C:22]([N:25]([CH3:27])[CH3:26])=[CH:21][CH:20]=2)=[CH2:18])=[CH:13][CH:12]=1)[CH3:9].[Cl:28][C:29]1[C:30]([Cl:42])=[C:31]([Cl:41])[C:32]([Cl:40])=[C:33]2[C:38](=O)[O:37][C:35](=[O:36])[C:34]=12.[OH-].[Na+]>O.ClC1C=CC=CC=1Cl>[CH3:27][N:25]([CH3:26])[C:22]1[CH:21]=[CH:20][C:19]([C:17]([C:14]2[CH:15]=[CH:16][C:11]([O:10][CH2:8][CH3:9])=[CH:12][CH:13]=2)=[CH:18][C:38]2([CH:18]=[C:17]([C:14]3[CH:13]=[CH:12][C:1]([O:4][CH2:5][CH3:6])=[CH:2][CH:15]=3)[C:19]3[CH:24]=[CH:23][C:22]([N:25]([CH3:27])[CH3:26])=[CH:21][CH:20]=3)[C:33]3[C:34](=[C:29]([Cl:28])[C:30]([Cl:42])=[C:31]([Cl:41])[C:32]=3[Cl:40])[C:35](=[O:36])[O:37]2)=[CH:24][CH:23]=1

参加物

7

反応物 4

HCID 7918Acetic AnhydrideHCID 8326Tetrachlorophthalic anhydrideHCID 14798Sodium HydroxideHCID 145122554-[1-(4-Ethoxyphenyl)ethenyl]-N,N-dimethylaniline

生成物 1

HCID 54074224HCID 54074224、化合物収率 80.8%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 72391,2-Dichlorobenzene溶媒

反応条件

温度
120 °C

実験手順

Into a mixture of 25 ml of acetic anhydride and 75 ml of o-dichlorobenzene, 13.4 g of 1-(p-ethoxyphenyl)-1-(p-dimethylaminophenyl)ethylene (melting at 110°-111° C.) and 21.5 g of tetrachlorophthalic anhydride were added and the mixture was stirred for 6 hours at 120° C. After adding the reaction mixture into 200 ml of water and making the mixture alkaline by sodium hydroxide, the alkaline mixture was extracted with 70 ml of toluene. The solid matter obtained by distilling off toluene from the extract was recrystallized from acetone while purifying with activated carbon to obtain 16.2 g of pale yellow crystals in a yield of 80.8%.

後処理

  1. additionwere added
  2. extractionthe alkaline mixture was extracted with 70 ml of toluene
  3. customThe solid matter obtained
  4. distillationby distilling off toluene from the extract
  5. customwas recrystallized from acetone
  6. customwhile purifying with activated carbon

出典と根拠

ORDレコード
ord-ec5b4c14384a4b7198296d0079296fdd
出典データセット
uspto-grants-1989_05
特許番号
US04835291

反応ノート

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