Benzene → HCID 15382032, 화합물

HRID 2380697노트

반응식

HRID 2380697 반응식
C1([C:7]2[CH:8]=[C:9]([CH:34]=[CH:35][CH:36]=2)[CH:10]=[CH:11][C:12]([N:14]2[CH2:19][CH2:18][N:17]([C:20](=[S:33])[C:21]3[CH:26]=[C:25]([O:27][CH3:28])[C:24]([O:29][CH3:30])=[C:23]([O:31][CH3:32])[CH:22]=3)[CH2:16][CH2:15]2)=O)C=CC=CC=1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:46])=CC=1.O.[CH:60]1[CH:65]=[CH:64][CH:63]=[CH:62][CH:61]=1>>[C:9]1([C:10]([C:60]2[CH:65]=[CH:64][CH:63]=[CH:62][CH:61]=2)=[CH:11][C:12]([N:14]2[CH2:15][CH2:16][N:17]([C:20](=[S:33])[C:21]3[CH:22]=[C:23]([O:31][CH3:32])[C:24]([O:29][CH3:30])=[C:25]([O:27][CH3:28])[CH:26]=3)[CH2:18][CH2:19]2)=[S:46])[CH:34]=[CH:35][CH:36]=[CH:7][CH:8]=1

참가 물질

5

반응물 4

HCID 241BenzeneHCID 962WaterHCID 87949Lawesson's reagent2회HCID 54370034HCID 54370034, 화합물

생성물 1

HCID 15382032HCID 15382032, 화합물

실험 절차

A solution of 1.000 g of 1-(3-phenylcinnamoyl)-4-[3,4,5-trimethoxy(thiobenzoyl)]piperazine (prepared as described in Example 61) in 10 ml of benzene and 0.805 g of Lawesson's Reagent [consisting mainly of [2,4-bis(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulfide] was heated under reflux for 2 hours. At the end of this time, the reaction mixture was cooled to room temperature, poured into water and extracted twice with ethyl acetate. The extract was washed with water, dried over anhydrous sodium sulfate, and concentrated by distillation under reduced pressure. The residue was purified by column chromatography through 30 g of silica gel eluted with a 3:1 by volume mixture of hexane and ethyl acetate, to give 1.010 g of the title compound as a yellow powder.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 2 hours
  3. extractionextracted twice with ethyl acetate
  4. washThe extract was washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated by distillation under reduced pressure
  7. customThe residue was purified by column chromatography through 30 g of silica gel
  8. washeluted with a 3:1 by volume mixture of hexane and ethyl acetate

출처 및 근거

ORD 기록
ord-706743a62c5a4209a98baeb64f8a674c
출처 데이터셋
uspto-grants-1994_11
특허 번호
US05369106

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