Water → HCID 22625603、化合物

HRID 1378954ノート

反応式

HRID 1378954 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]1[N:10]=[C:11]2[CH2:16][CH2:15][CH2:14][CH2:13][N:12]2[CH:17]=1.[Cl:18]N1C(=O)CCC1=O.O.CCCCCC.C(OCC)(=O)C>CN(C)C=O>[Cl:18][C:17]1[N:12]2[CH2:13][CH2:14][CH2:15][CH2:16][C:11]2=[N:10][C:9]=1[C:3]1[CH:4]=[CH:5][C:6]([Cl:8])=[CH:7][C:2]=1[Cl:1]

参加物

6

反応物 4

HCID 962WaterHCID 31398ChlorosuccinimideHCID 21226206Ethyl acetate hexane2 回HCID 22625614HCID 22625614、化合物

生成物 1

HCID 22625603HCID 22625603、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
70 °C

実験手順

A mixture of 1.0 g (3.7 mmol) of 2-(2,4-dichlorophenyl)-5,6,7,8-tetrahydroimidazo[1,2-a]pyridine and 0.6 g (4.5 mmol) of N-chlorosuccinimide was stirred in 15 ml of dimethylformamide at room temperature overnight followed by heating at 70° C. for 20 minutes. An excess of water was added and the aqueous mixture extracted with 200 ml of ethyl acetate. The separated organic layer layer was washed with water, saturated aqueous sodium bicarbonate, and brine. After drying over magnesium sulfate, the solvent was removed in vacuo to give a oily residue. Silica gel column chromatography (3:1 followed by 1:1 hexane/ethyl acetate followed in turn by 2:1 ethyl acetate/hexane) afforded the title compound as the main component (0.65 g, m.p. 99°-101° C.).

後処理

  1. extractionthe aqueous mixture extracted with 200 ml of ethyl acetate
  2. washThe separated organic layer layer was washed with water, saturated aqueous sodium bicarbonate, and brine
  3. dry with materialAfter drying over magnesium sulfate
  4. customthe solvent was removed in vacuo
  5. customto give a oily residue

出典と根拠

ORDレコード
ord-2aafee31de5049b184871248edf8debe
出典データセット
uspto-grants-1997_09
特許番号
US05670455

反応ノート

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