Acetonitrile → HCID 12004101、化合物

HRID 971258ノート

反応式

HRID 971258 の反応式
Cl[C:2]1[C:3]2[CH2:11][CH2:10][N:9]([C:12]3[C:17]([Cl:18])=[CH:16][CH:15]=[CH:14][N:13]=3)[CH2:8][C:4]=2[N:5]=[CH:6][N:7]=1.[NH2:19][C:20]1[CH:28]=[C:27]2[C:23]([C:24]([CH3:33])([CH3:32])[CH2:25][N:26]2[C:29](=[O:31])[CH3:30])=[CH:22][CH:21]=1.C(#N)C.C(=O)(O)[O-].[Na+]>CCOC(C)=O>[Cl:18][C:17]1[C:12]([N:9]2[CH2:10][CH2:11][C:3]3[C:2]([NH:19][C:20]4[CH:28]=[C:27]5[C:23]([C:24]([CH3:33])([CH3:32])[CH2:25][N:26]5[C:29](=[O:31])[CH3:30])=[CH:22][CH:21]=4)=[N:7][CH:6]=[N:5][C:4]=3[CH2:8]2)=[N:13][CH:14]=[CH:15][CH:16]=1

参加物

6

反応物 4

HCID 6342AcetonitrileHCID 516892Sodium BicarbonateHCID 218651761-(6-Amino-3,3-dimethylindolin-1-yl)ethanoneHCID 590214784-Chloro-7-(3-chloropyridin-2-yl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidine

生成物 1

HCID 12004101HCID 12004101、化合物収率 79.6%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
180 °C

実験手順

A mixture of 4-chloro-7-(3-chloropyridin-2-yl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidine (40 mg, 0.14 mmol), 1-(6-amino-3,3-dimethylindolin-1-yl)ethanone (60 mg, 0.29 mmol), and acetonitrile (3 mL) was heated in a sealed tube via microwave at 180° C. for 60 min. The mixture was treated with EtOAc (50 mL) and saturated aqueous sodium bicarbonate. The organic layer was separated and washed with brine, dried (Na2SO4), and evaporated. The residue was purified by flash chromatography over silica gel to give an off-white solid (50 mg).

後処理

  1. customThe organic layer was separated
  2. washwashed with brine
  3. dry with materialdried (Na2SO4)
  4. customevaporated
  5. customThe residue was purified by flash chromatography over silica gel

出典と根拠

ORDレコード
ord-412e5b5c6c0e4f23b1cad564a8d9fc7b
出典データセット
uspto-grants-2007_12
特許番号
US07312330B2

反応ノート

読み込み中…