Acetic Anhydride → HCID 54074224, 화합물

HRID 1763169노트

반응식

HRID 1763169 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

HCID 54074224HCID 54074224, 화합물수율 80.8%

시약·촉매·용매 2

HCID 962Water용매HCID 72391,2-Dichlorobenzene용매

반응 조건

온도
120 °C

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-ec5b4c14384a4b7198296d0079296fdd
출처 데이터셋
uspto-grants-1989_05
특허 번호
US04835291

반응 노트

불러오는 중…