Dichloromethane → HCID 14156369、化合物

HRID 1253264

反応式

HRID 1253264 の反応式
[CH:1]12[C:9](=[O:10])[O:8][C:6](=O)[CH:3]([CH2:4][CH2:5]1)[CH2:2]2.[NH2:11][CH2:12][CH2:13][CH2:14][CH2:15][N:16]1[CH2:21][CH2:20][N:19]([C:22]2[CH:27]=[CH:26][CH:25]=[C:24]([Cl:28])[CH:23]=2)[CH2:18][CH2:17]1.C(Cl)Cl.C1(C)C(C)=CC=CC=1>O>[Cl:28][C:24]1[CH:23]=[C:22]([N:19]2[CH2:18][CH2:17][N:16]([CH2:15][CH2:14][CH2:13][CH2:12][N:11]3[C:6](=[O:8])[CH:3]4[CH2:2][CH:1]([CH2:5][CH2:4]4)[C:9]3=[O:10])[CH2:21][CH2:20]2)[CH:27]=[CH:26][CH:25]=1

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 7237O-XyleneHCID 2397991,3-Cyclopentanedicarboxylic anhydrideHCID 128407044-[4-(3-Chlorophenyl)piperazin-1-yl]butan-1-amine

生成物 1

HCID 14156369HCID 14156369、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

1,3-Cyclopentane dicarboxylic anhydride (2.2 g., 15 mmole) and 4.0 g. (15 mmole) of 1-(4-aminobutyl)-4-(3-chlorophenyl)piperazine were combined in 300 ml. of methylene chloride and stirred for 30 minutes at room temperature. The solvent was replaced with xylene and the mixture was refluxed for 48 hours with water removal via a Dean-Stark trap. The solvent was removed in vacuum and the residue filtered through 75 g. of silica gel with 2% ethanol/chloroform as eluent. The product was concentrated in vacuum and crystallized from 50 ml. of isopropanol with addition of 4N isopropanolic HCl. Recrystallization from ethanol gave 1.6 g. of the title compound as the hydrochloride, quarter hydrate; m.p. 199°-202° C.

後処理

  1. customThe solvent was removed in vacuum
  2. filtrationthe residue filtered through 75 g
  3. concentrationThe product was concentrated in vacuum
  4. customcrystallized from 50 ml
  5. additionof isopropanol with addition of 4N isopropanolic HCl
  6. customRecrystallization from ethanol
  7. customgave 1.6 g

出典と根拠

ORDレコード
ord-0414f49d39d6428e8394f535d7f0ce73
出典データセット
uspto-grants-1988_05
特許番号
US04748240

関連ノート

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