Hydrochloric Acid → cis-2-[4-[4-(6-Fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]butyl]hexahydro-1H-isoindole-1,3-dione hydrochloride

HRID 264194

反応式

HRID 264194 の反応式
[NH2:1][CH2:2][CH2:3][CH2:4][CH2:5][N:6]1[CH2:11][CH2:10][CH:9]([C:12]2[C:16]3[CH:17]=[CH:18][C:19]([F:21])=[CH:20][C:15]=3[O:14][N:13]=2)[CH2:8][CH2:7]1.[C@@H:22]12[C:31](=O)[O:30][C:28](=[O:29])[C@@H:23]1[CH2:24][CH2:25][CH2:26][CH2:27]2.[ClH:33]>N1C=CC=CC=1.C(O)C>[ClH:33].[F:21][C:19]1[CH:18]=[CH:17][C:16]2[C:12]([CH:9]3[CH2:10][CH2:11][N:6]([CH2:5][CH2:4][CH2:3][CH2:2][N:1]4[C:28](=[O:29])[C@H:23]5[C@H:22]([CH2:27][CH2:26][CH2:25][CH2:24]5)[C:31]4=[O:30])[CH2:7][CH2:8]3)=[N:13][O:14][C:15]=2[CH:20]=1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 641660Hexahydrophthalic anhydride, cis-HCID 219600491-(4-Aminobutyl)-4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidine

生成物 1

HCID 67071030cis-2-[4-[4-(6-Fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]butyl]hexahydro-1H-isoindole-1,3-dione hydrochloride

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒2 回HCID 1049Pyridine溶媒2 回

実験手順

A mixture of 1-(4-aminobutyl)-4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidine (4.7 g, 16.1 mmol) and cis-1,2-cyclohexanedicarboxylic anhydride (3.23 g, 21 mmol) in pyridine (45 ml) was heated at reflux for 8 hours. At the end of the reaction, pyridine was removed to dryness. The crude product was purified on a silica gel column. The material thus obtained weighed 3.18 g (45%) as a clear oil. This oil was dissolved in ethanol (15 ml), then was treated with HCl in ethanol (45 ml). Crystallization took place upon cooling. The crystals were collected, 3.2 g, m.p.=229°-231° C.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 8 hours
  3. customwas removed to dryness
  4. customThe crude product was purified on a silica gel column
  5. customThe material thus obtained
  6. customCrystallization
  7. temperatureupon cooling
  8. customThe crystals were collected

出典と根拠

ORDレコード
ord-c44d6f4fc14348bda8125badb1b1eabb
出典データセット
uspto-grants-1997_07
特許番号
US05646161

関連ノート

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