Sodium Iodide → HCID 57917660、化合物

HRID 1878433ノート

反応式

HRID 1878433 の反応式
Cl[CH2:2][C:3]1[CH:4]=[C:5]([CH:15]=[CH:16][CH:17]=1)[C:6]([NH:8][CH:9]1[CH2:12][C:11]([F:14])([F:13])[CH2:10]1)=[O:7].[N:18]1([C:24]([O:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[O:25])[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]1.C(=O)([O-])[O-].[K+].[K+].[I-].[Na+]>C(#N)C>[F:13][C:11]1([F:14])[CH2:12][CH:9]([NH:8][C:6]([C:5]2[CH:4]=[C:3]([CH:17]=[CH:16][CH:15]=2)[CH2:2][N:21]2[CH2:20][CH2:19][N:18]([C:24]([O:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[O:25])[CH2:23][CH2:22]2)=[O:7])[CH2:10]1

参加物

6

反応物 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 143452tert-Butyl piperazine-1-carboxylateHCID 668783523-(chloromethyl)-N-(3,3-difluorocyclobutyl)benzamide

生成物 1

HCID 57917660HCID 57917660、化合物収率 98.7%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

3-(Chloromethyl)-N-(3,3-difluorocyclobutyl)benzamide (12.82 mmol, 3.33 g), tert-butyl piperazine-1-carboxylate (12.82 mmol, 2.388 g), potassium carbonate (38.5 mmol, 5.32 g) and sodium iodide (2.56 mmol, 0.384 g) were combined and heated at reflux in acetonitrile (50 ml) for 2 hours. The solvent was removed under reduced pressure and the residue taken up in dichloromethane, washed with water, dried over sodium sulfate and concentrated under vacuum to afford the title compound (5.179 g).

後処理

  1. temperatureheated
  2. customThe solvent was removed under reduced pressure
  3. washwashed with water
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-97e3627ab6f8437cb5236f74099bc6a5
出典データセット
uspto-grants-2012_11
特許番号
US08314091B2

反応ノート

読み込み中…