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Acetic Anhydride → HCID 54573772, 화합물

HRID 1382839
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HRID 1382839 반응식
[C:1]([O:4][C:5](=O)[CH3:6])(=O)C.[CH3:8][O:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]([C:18]2[CH:23]=[CH:22][C:21]([N:24]3[CH2:28][CH2:27][CH2:26][CH2:25]3)=[CH:20][CH:19]=2)=[CH2:17])=[CH:12][CH:11]=1.[Cl:29][C:30]1[C:31]([Cl:43])=[C:32]([Cl:42])[C:33]([Cl:41])=[C:34]2[C:39](=O)[O:38][C:36](=[O:37])[C:35]=12.[OH-].[Na+]>O.ClC1C=CC=CC=1Cl>[N:24]1([C:21]2[CH:22]=[CH:23][C:18]([C:16]([C:13]3[CH:14]=[CH:15][C:10]([O:9][CH3:8])=[CH:11][CH:12]=3)=[CH:17][C:39]3([CH:17]=[C:16]([C:13]4[CH:14]=[CH:6][C:5]([O:4][CH3:1])=[CH:11][CH:12]=4)[C:18]4[CH:23]=[CH:22][C:21]([N:24]5[CH2:28][CH2:27][CH2:26][CH2:25]5)=[CH:20][CH:19]=4)[C:34]4[C:35](=[C:30]([Cl:29])[C:31]([Cl:43])=[C:32]([Cl:42])[C:33]=4[Cl:41])[C:36](=[O:37])[O:38]3)=[CH:19][CH:20]=2)[CH2:28][CH2:27][CH2:26][CH2:25]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 7918Acetic AnhydrideHCID 8326Tetrachlorophthalic anhydrideHCID 14798Sodium HydroxideHCID 143237921-{4-[1-(4-Methoxyphenyl)ethenyl]phenyl}pyrrolidine

생성물 1

HCID 54573772HCID 54573772, 화합물수율 85.2%

시약·촉매·용매 2

HCID 962
Water
용매
HCID 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, 14.0 g of 1-(p-methoxyphenyl)-1-(p-pyrrolidinophenyl)ethylene (m.p. 115°-118° C.) and 21.5 g of tetrachlorophthalic anhydride were added and the mixture was stirred for 6 hours at 120° C. Into 200 ml of water the reaction mixture was added and after making the mixture alkaline by adding sodium hydroxide, the alkaline reaction mixture was extracted with 70 ml of toluene. The solid matter obtained by evaporating toluene from the extract was recrystallized from acetone while purifying with activated carbon to obtain 17.6 g of pale yellow crystals melting at 159° to 161° C. (Yield: 85.2%)

후처리

  1. additionwere added
  2. customthe alkaline reaction mixture
  3. extractionwas extracted with 70 ml of toluene
  4. customThe solid matter obtained
  5. customby evaporating toluene from the extract
  6. customwas recrystallized from acetone
  7. customwhile purifying with activated carbon

출처 및 근거

ORD 기록
ord-69037fed5edf4976bc7054704dc7f054
출처 데이터셋
uspto-grants-1989_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04808567

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