Benzene → HCID 15382032、化合物

HRID 2380697ノート

反応式

HRID 2380697 の反応式
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

参加物

5

反応物 4

HCID 241BenzeneHCID 962WaterHCID 87949Lawesson's reagent2 回HCID 54370034HCID 54370034、化合物

生成物 1

HCID 15382032HCID 15382032、化合物

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-706743a62c5a4209a98baeb64f8a674c
出典データセット
uspto-grants-1994_11
特許番号
US05369106

反応ノート

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