Citric Acid → HCID 609964、化合物

HRID 349733ノート

反応式

HRID 349733 の反応式
F[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[NH:11][C:12](=[O:14])[CH3:13].[NH:15]1[CH2:19][CH2:18][CH2:17][CH2:16]1.C(O)(=O)CC(CC(O)=O)(C(O)=O)O>ClCCl>[N+:8]([C:5]1[CH:6]=[CH:7][C:2]([N:15]2[CH2:19][CH2:18][CH2:17][CH2:16]2)=[C:3]([NH:11][C:12](=[O:14])[CH3:13])[CH:4]=1)([O-:10])=[O:9]

参加物

5

反応物 3

HCID 311Citric AcidHCID 31268PyrrolidineHCID 2779405N-(2-fluoro-5-nitrophenyl)acetamide

生成物 1

HCID 609964HCID 609964、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
90 °C

実験手順

0.5 g (2.5 mmol) of N-(2-fluoro-5-nitrophenyl)acetamide was admixed in a pressure reaction vessel with 1 ml (12.6 mmol) of pyrrolidine and stirred at 90° C. for 2.5 hours. After the mixture had been cooled, it was diluted with 20 ml of dichloromethane, adjusted to pH 4 using citric acid solution (10%) and washed four times with water. After the organic phase had been dried, the solvent was removed under reduced pressure. In the aqueous phase, a solid is precipitated out. It was filtered off with suction and washed with water, and combined with the residue from the organic phase (yield 0.58 g, 93%). The product was reacted in stage c without further purification.

後処理

  1. temperatureAfter the mixture had been cooled
  2. washwashed four times with water
  3. customAfter the organic phase had been dried
  4. customthe solvent was removed under reduced pressure
  5. customIn the aqueous phase, a solid is precipitated out
  6. filtrationIt was filtered off with suction
  7. washwashed with water
  8. customThe product was reacted in stage c without further purification

出典と根拠

ORDレコード
ord-a3e8ed503ed24238a144129b55c1b3fd
出典データセット
uspto-grants-2007_02
特許番号
US07179941B2

反応ノート

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