3-(4-(2-Chlorophenyl)piperazin-1-yl)propan-1-ol → HCID 131718161、化合物

HRID 5847

反応式

HRID 5847 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([N:13]=[C:14]=[O:15])[CH:6]=[C:7]([O:11][CH3:12])[C:8]=1[O:9][CH3:10].[Cl:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=1[N:23]1[CH2:28][CH2:27][N:26]([CH2:29][CH2:30][CH2:31][OH:32])[CH2:25][CH2:24]1>C1(C)C=CC=CC=1>[ClH:16].[Cl:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=1[N:23]1[CH2:24][CH2:25][N:26]([CH2:29][CH2:30][CH2:31][O:32][C:14](=[O:15])[NH:13][C:5]2[CH:6]=[C:7]([O:11][CH3:12])[C:8]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:4]=2)[CH2:27][CH2:28]1

参加物

4

反応物 2

HCID 2432883-(4-(2-Chlorophenyl)piperazin-1-yl)propan-1-olHCID 5177665-Isocyanato-1,2,3-trimethoxybenzene

生成物 1

HCID 131718161HCID 131718161、化合物収率 40%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of 3,4,5-trimethoxyphenylisocyanate (420 mg; 2.0 mmol) (produced as in Example 1) and 3-[4-(2-chloro-phenyl) -1-piperazinyl]propanol (500 mg; 20 mmol) in toluene (25 ml) was refluxed for 16 h. The solvent was evaporated and the residue taken up in ethanol, which was treated with hydrogen chloride in ether. Recrystallization from ethanol/ether afforded 400 mg of the title compound. M.p. 185°-187° C. MS (70 eV): m/z 463 (6%, M+), 254 (30), 209 (100), 194 (52), 166 (34), 70 (58).

後処理

  1. temperaturewas refluxed for 16 h
  2. customThe solvent was evaporated
  3. additionwhich was treated with hydrogen chloride in ether
  4. customRecrystallization from ethanol/ether

出典と根拠

ORDレコード
ord-dca1c35f5eed401ebd1117828fd2510f
出典データセット
uspto-grants-1993_09
特許番号
US05246935

関連ノート

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