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Methanol → 7-ethynyl-4H-imidazo[2,1-c][1,4]benzoxazine

HRID 2035690
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반응식

HRID 2035690 반응식
[CH:1]1[N:9]2[C:4]([CH2:5][O:6][C:7]3[CH:13]=[C:12]([CH:14]=O)[CH:11]=[CH:10][C:8]=32)=[N:3][CH:2]=1.[C:16](=O)([O-])[O-].[K+].[K+].CO>C(Cl)Cl>[C:14]([C:12]1[CH:11]=[CH:10][C:8]2[N:9]3[CH:1]=[CH:2][N:3]=[C:4]3[CH2:5][O:6][C:7]=2[CH:13]=1)#[CH:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 887MethanolHCID 11430Potassium CarbonateHCID 866614644H-Benzo[b]imidazo[1,2-d][1,4]oxazine-7-carbaldehyde

생성물 1

HCID 580636067-ethynyl-4H-imidazo[2,1-c][1,4]benzoxazine수율 43.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

4H-Imidazo[2,1-c][1,4]benzoxazine-7-carbaldehyde (44 mg, 0.140 mmol) and anhydrous potassium carbonate (120 mg, 0.868 mmol) were placed in a 25-ml flask and placed on high vacuum for 10 min. Under N2, anhydrous MeOH (5 ml) was added. To the suspension was added dimethyl (1-diazo-2-oxopropyl) phosphonate (0.03 ml, 0.192 mmol). The reaction was stirred at rt for 2 h. The mixture was diluted with DCM, washed with water, dried over sodium sulfate, concentrated to afford desired product (11.9 mg, 0.061 mmol, 43.3% yield).

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후처리

  1. washwashed with water
  2. dry with materialdried over sodium sulfate
  3. concentrationconcentrated

출처 및 근거

ORD 기록
ord-4bda9907f1be46018a5c9c67bb03cc76
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08575150B2

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