Water → 2-[4-(4-Chlorophenyl)-1H-imidazol-2-yl]-4-(phenylmethyl)morpholine

HRID 2367336ノート

反応式

HRID 2367336 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=O)[CH2:9][NH:10][C:11]([CH:13]2[O:18][CH2:17][CH2:16][N:15]([CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[CH2:14]2)=O)=[CH:4][CH:3]=1.FC(F)(F)C([O-])=O.[NH4+:34].O>C(Cl)Cl>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:34]=[C:11]([CH:13]3[O:18][CH2:17][CH2:16][N:15]([CH2:19][C:20]4[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=4)[CH2:14]3)[NH:10][CH:9]=2)=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 962WaterHCID 2724268Ammonium trifluoroacetateHCID 58504731N-[2-(4-Chlorophenyl)-2-oxoethyl]-4-(phenylmethyl)-2-morpholinecarboxamide

生成物 1

HCID 1784779552-[4-(4-Chlorophenyl)-1H-imidazol-2-yl]-4-(phenylmethyl)morpholine収率 89.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
150 °C

実験手順

A mixture of N-[2-(4-chlorophenyl)-2-oxoethyl]-4-(phenylmethyl)-2-morpholinecarboxamide (3.3 g, 8.85 mmol) and ammonium trifluoroacetate (5.27 g, 44.3 mmol) was heated at 150° C. for 20 minutes. After cooling, to the resulting mixture was added water (50 mL) and CH2Cl2 (50 mL). The organic layer was separated and washed with brine, dried (MgSO4), and concentrated to afford the crude title compound (2.8 g). LC-MS (ES) m/z=354 [M+H]+.

後処理

  1. temperatureAfter cooling, to the resulting mixture
  2. customThe organic layer was separated
  3. washwashed with brine
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-14059799eabe4bb2aa328720fd0d7674
出典データセット
uspto-grants-2014_04
特許番号
US08697685B2

反応ノート

読み込み中…