Chloroacetamide → Tert-butyl 4-(2-carbamoylbenzofuran-5-yl)piperazine-1-carboxylate

HRID 1883956

反応式

HRID 1883956 の反応式
Cl[CH2:2][C:3]([NH2:5])=[O:4].C(=O)([O-])[O-].[K+].[K+].[C:12]([O:16][C:17]([N:19]1[CH2:24][CH2:23][N:22]([C:25]2[CH:26]=[CH:27][C:28]([OH:33])=[C:29]([CH:32]=2)[CH:30]=O)[CH2:21][CH2:20]1)=[O:18])([CH3:15])([CH3:14])[CH3:13]>CN1CCCC1=O>[C:12]([O:16][C:17]([N:19]1[CH2:20][CH2:21][N:22]([C:25]2[CH:26]=[CH:27][C:28]3[O:33][C:2]([C:3]([NH2:5])=[O:4])=[CH:30][C:29]=3[CH:32]=2)[CH2:23][CH2:24]1)=[O:18])([CH3:15])([CH3:13])[CH3:14]

参加物

5

反応物 3

HCID 6580ChloroacetamideHCID 11430Potassium CarbonateHCID 23508726tert-Butyl 4-(3-formyl-4-hydroxyphenyl)piperazine-1-carboxylate

生成物 1

HCID 11244883Tert-butyl 4-(2-carbamoylbenzofuran-5-yl)piperazine-1-carboxylate

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
60 °C

実験手順

5 ml of 1-methyl-2-pyrrolidone, 0.16 g of chloroacetamide and 0.25 g of potassium carbonate are added at 20° C. with stirring/under nitrogen to 0.5 g of 5-(4-tert-butoxycarbonylpiperazin-1-yl)-2-hydroxybenzaldehyde. The mixture is stirred at 60° C. for 16 hours, cooled and then filtered, and the solvent is removed under reduced pressure. The residue is taken up in MTB ether, re-filtered and concentrated, and the residue is crystallized from toluene. The isolated yield is 0.34 g (60%).

後処理

  1. temperaturecooled
  2. filtrationfiltered
  3. customthe solvent is removed under reduced pressure
  4. filtrationre-filtered
  5. concentrationconcentrated
  6. customthe residue is crystallized from toluene

出典と根拠

ORDレコード
ord-18960a06f803452e8e3f8345adf75c2b
出典データセット
uspto-grants-2004_07
特許番号
US06762300B2

関連ノート

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