Potassium Carbonate → HCID 78992995、化合物

HRID 1504595ノート

反応式

HRID 1504595 の反応式
Cl[C:2]1[CH:10]=[CH:9][C:5]([C:6]([NH2:8])=[O:7])=[CH:4][N:3]=1.[NH:11]1[CH2:14][CH:13]([OH:15])[CH2:12]1.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[OH:15][CH:13]1[CH2:14][N:11]([C:2]2[CH:10]=[CH:9][C:5]([C:6]([NH2:8])=[O:7])=[CH:4][N:3]=2)[CH2:12]1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 804566-ChloronicotinamideHCID 15142903-Hydroxyazetidine

生成物 1

HCID 78992995HCID 78992995、化合物収率 25.9%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
125 °C

実験手順

To a solution of 6-chloronicotinamide (0.16 g, 1 mmol) and azetidin-3-ol (73 mg, 1 mmol) in DMF (5 ml) under nitrogen was added K2CO3 (0.41 g, 3 mmol). The resulting solution was stirred under nitrogen at 125° C. for 24 h. After all the starting materials were consumed, the reaction mixture was allowed to cool to ambient temperature. The reaction mixture was then filtered and the filter cake was washed with ethyl acetate. The combined filtrates were concentrated to afford the title compound (50 mg, 25%) as a yellow solid. [LCMS RtA=0.81 min, [M+H]+=194.1].

後処理

  1. customAfter all the starting materials were consumed
  2. temperatureto cool to ambient temperature
  3. filtrationThe reaction mixture was then filtered
  4. washthe filter cake was washed with ethyl acetate
  5. concentrationThe combined filtrates were concentrated

出典と根拠

ORDレコード
ord-df7dc700cbb94f0fae475e32b9162eb5
出典データセット
uspto-grants-2015_12
特許番号
US09216182B2

反応ノート

読み込み中…