Diisopropylethylamine → 3-[4-(2-Bromo-5-fluorophenoxy)piperidin-1-yl]-4,5-dihydroisoxazole-5-carboxamide

HRID 561207ノート

反応式

HRID 561207 の反応式
Br[C:2]1[CH2:6][CH:5]([C:7]([NH2:9])=[O:8])[O:4][N:3]=1.[Br:10][C:11]1[CH:23]=[CH:22][C:21]([F:24])=[CH:20][C:12]=1[O:13][CH:14]1[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1.C(N(CC)C(C)C)(C)C>C(O)C>[Br:10][C:11]1[CH:23]=[CH:22][C:21]([F:24])=[CH:20][C:12]=1[O:13][CH:14]1[CH2:15][CH2:16][N:17]([C:2]2[CH2:6][CH:5]([C:7]([NH2:9])=[O:8])[O:4][N:3]=2)[CH2:18][CH2:19]1

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 441183083-Bromo-4,5-dihydro-1,2-oxazole-5-carboxamideHCID 578327574-(2-Bromo-5-fluorophenoxy)piperidine

生成物 1

HCID 666968003-[4-(2-Bromo-5-fluorophenoxy)piperidin-1-yl]-4,5-dihydroisoxazole-5-carboxamide

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 3-bromo-4,5-dihydroisoxazole-5-carboxamide (1.5 g, 7.77 mmol), 4-(2-bromo-5-fluorophenoxy)piperidine (2.56 g, 9.33 mmol) and N,N-diisopropylethylamine (3.5 mL, 20.04 mmol) in ethanol (15 mL) was heated at reflux temperature overnight. Solvent was then removed in vacuo. The residue was suspended in water and stirred for 1 h. The solid was collected, washed with water and Et2O. Drying under vacuum gave the title compound as a light brown powder.

後処理

  1. temperaturewas heated
  2. temperatureat reflux temperature overnight
  3. customSolvent was then removed in vacuo
  4. customThe solid was collected
  5. washwashed with water and Et2O
  6. customDrying under vacuum

出典と根拠

ORDレコード
ord-b38cba21652543928f35c93aff5fce0f
出典データセット
uspto-grants-2011_11
特許番号
US08063224B2

反応ノート

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