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Ammonia → HCID 67363450, 화합물

HRID 245771
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HRID 245771 반응식
[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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 222AmmoniaHCID 21584119Ethylacetate methanolHCID 67362972HCID 67362972, 화합물

생성물 1

HCID 67363450HCID 67363450, 화합물수율 108.8%

시약·촉매·용매 2

HCID 887Methanol용매HCID 86584057Phosphorus Pentoxide-Methanesulfonic Acid용매

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온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-318bd86d40564d8cbb1e31a6f71149c2
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08658794B2

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