Ammonium trifluoroacetate → 2-[4-(3-Chlorophenyl)-1H-imidazol-2-yl]-4-(phenylmethyl)morpholine

HRID 2367358ノート

反応式

HRID 2367358 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([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:5]=[CH:6][CH:7]=1.FC(F)(F)C([O-])=O.[NH4+:34]>O>[Cl:1][C:2]1[CH:3]=[C:4]([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:5]=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 2724268Ammonium trifluoroacetateHCID 66990931N-[2-(3-Chlorophenyl)-2-oxoethyl]-4-(phenylmethyl)-2-morpholinecarboxamide

生成物 1

HCID 1784780512-[4-(3-Chlorophenyl)-1H-imidazol-2-yl]-4-(phenylmethyl)morpholine収率 96.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
150 °C

実験手順

A mixture of N-[2-(3-chlorophenyl)-2-oxoethyl]-4-(phenylmethyl)-2-morpholinecarboxamide (350 mg, 0.939 mmol) and ammonium trifluoroacetate (615 mg, 4.69 mmol) was stirred for 2.5 hours at 150° C. Water (150 mL) was added to the residue, and the aqueous mixture was extracted with EtOAc (200 mL). The organic phase was dried (Na2SO4), filtered, and concentrated to afford the title compound (320 mg) as a brown oil. LC-MS (ES) m/z=354 [M+H]+.

後処理

  1. extractionthe aqueous mixture was extracted with EtOAc (200 mL)
  2. dry with materialThe organic phase was dried (Na2SO4)
  3. filtrationfiltered
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-4d37e945ee9b4594a22f0b37a12f44c9
出典データセット
uspto-grants-2014_04
特許番号
US08697685B2

反応ノート

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