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Ammonia → HCID 67363450、化合物

HRID 245771
ノート
印刷プレビュー

反応式

HRID 245771 の反応式
[CH3:1][N:2]1[C:6](=[O:7])[CH2:5][CH:4]([C:8]([NH:10][CH2:11][C:12]2[C:17]([CH3:18])=[N:16][CH:15]=[CH:14][N:13]=2)=O)[CH2:3]1.N.C(OCC)(=O)C.CO>CS(O)(=O)=O.O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.CO>[CH3:1][N:2]1[CH2:3][CH:4]([C:8]2[N:13]3[CH:14]=[CH:15][N:16]=[C:17]([CH3:18])[C:12]3=[CH:11][N:10]=2)[CH2:5][C:6]1=[O:7]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 222AmmoniaHCID 21584119Ethylacetate methanolHCID 67362972HCID 67362972、化合物

生成物 1

HCID 67363450HCID 67363450、化合物収率 108.8%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 86584057Phosphorus Pentoxide-Methanesulfonic Acid溶媒

反応条件

温度
60 °C

実験手順

1-Methyl-N-((3-methylpyrazin-2-yl)methyl)-5-oxopyrrolidine-3-carboxamide (330 mg, 1.329 mmol) was dissolved in Eaton's reagent (2 ml) and the reaction mixture was stirred at 60° C. for 18 hour. Then the reaction mixture was poured into an ice-bath and basified with 7N ammonia in methanol (20 ml). The resulting mixture was extrated with chloroform/iso-propanol (9/1) five times. The combined organic extracts were dried (Na2SO4) and concentrated in vacuo. The residue (280 mg) was stripped with toluene twice and with dichloromethane twice. An additional crop (53 mg) was obtained by extraction of the water layer with chloroform/iso-propanol (9/1) twice and drying and concentrating as described before. In total 333 mg of crude 1-methyl-4-(8-methylimidazo[1,5-a]pyrazin-3-yl)pyrrolidin-2-one was obtained which was used in the next reaction without further purification.

後処理

  1. additionThen the reaction mixture was poured into an ice-bath
  2. dry with materialThe combined organic extracts were dried (Na2SO4)
  3. concentrationconcentrated in vacuo
  4. customAn additional crop (53 mg) was obtained by extraction of the water layer with chloroform/iso-propanol (9/1) twice
  5. customdrying
  6. concentrationconcentrating

出典と根拠

ORDレコード
ord-318bd86d40564d8cbb1e31a6f71149c2
出典データセット
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08658794B2

反応ノート

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