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Water → HCID 19972395、化合物

HRID 1452334
ノート
印刷プレビュー

反応式

HRID 1452334 の反応式
[Cl:1][CH2:2][CH2:3][CH2:4][S:5]([C:8]1[C:17]2[O:16][C:15]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[C:14]([CH3:24])[C:13](=[O:25])[C:12]=2[CH:11]=[CH:10][CH:9]=1)(=[O:7])=[O:6].[CH3:26][O:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=1[N:34]1[CH2:39][CH2:38][NH:37][CH2:36][CH2:35]1.O>CN(C)C=O>[ClH:1].[CH3:26][O:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=1[N:34]1[CH2:39][CH2:38][N:37]([CH2:2][CH2:3][CH2:4][S:5]([C:8]2[C:17]3[O:16][C:15]([C:18]4[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=4)=[C:14]([CH3:24])[C:13](=[O:25])[C:12]=3[CH:11]=[CH:10][CH:9]=2)(=[O:7])=[O:6])[CH2:36][CH2:35]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 13461-(2-Methoxyphenyl)piperazineHCID 19972358HCID 19972358、化合物

生成物 1

HCID 19972395HCID 19972395、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 3.8 g of Intermediate XXXV and 4 g of 1-(2-methoxyphenyl)-piperazine in 40 ml of dimethylformamide was heated at 60° C. for 7 hours. After cooling to 20°-25° C., the reaction mixture was poured into 500 ml of water and extracted with dichloromethane. The organic extracts were washed with water and dried on anhydrous sodium sulfate, and the solvent was then evaporated off in vacuo. The residue was purified by flash chromatography on silica gel, eluting with ethyl acetate: petroleum ether (1:1). The base of the title compound was obtained. It was dissolved in ethanol and one equivalent of ethanolic hydrogen chloride was added to give 4.5 g of the title compound, m.p. (215) 226°-228° C.

後処理

  1. temperatureAfter cooling to 20°-25° C.
  2. extractionextracted with dichloromethane
  3. washThe organic extracts were washed with water
  4. dry with materialdried on anhydrous sodium sulfate
  5. customthe solvent was then evaporated off in vacuo
  6. customThe residue was purified by flash chromatography on silica gel
  7. washeluting with ethyl acetate: petroleum ether (1:1)

出典と根拠

ORDレコード
ord-f027b1473f6b46788c36c93b95bef43d
出典データセット
uspto-grants-1997_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05605896

反応ノート

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