Furfurylamine → HCID 68276609、化合物

HRID 1400311ノート

反応式

HRID 1400311 の反応式
[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH2:6][NH2:7].[Br:8][C:9]([F:16])([F:15])[C:10](OCC)=[O:11].C([O-])([O-])=O.[K+].[K+]>CN(C=O)C.O>[Br:8][C:9]([F:16])([F:15])[C:10]([NH:7][CH2:6][C:2]1[O:1][CH:5]=[CH:4][CH:3]=1)=[O:11]

参加物

6

反応物 3

HCID 3438FurfurylamineHCID 11430Potassium CarbonateHCID 69585Ethyl bromodifluoroacetate

生成物 1

HCID 68276609HCID 68276609、化合物収率 88%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 1-(furan-2-yl)methanamine (1 g, 10.3 mmol) in 15 mL of dry DMF, ethyl bromo(difluoro)acetate (2.3 g, 11.3 mmol) and K2CO3 (2.13 g, 15.4 mmol) were added. The solution was stirred for 18 h at room temperature. The mixture was diluted with 30 mL of water and extracted with 2×20 mL of ethyl acetate. The organic layer was dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo to afford 2-bromo-2,2-difluoro-N-(furan-2-ylmethyl)acetamide as red oil (2.3 g, 88% yield). HPLC-MS (ESI+): m/z 255.03 [M+H+].

後処理

  1. extractionextracted with 2×20 mL of ethyl acetate
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-2b8fcca4d09445f9832331aa8164cfe5
出典データセット
uspto-grants-2014_12
特許番号
US08906946B2

反応ノート

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