Sodium Methoxide → HCID 59312304, 화합물

HRID 2077057노트

반응식

HRID 2077057 반응식
[CH2:1]([N:8]1[CH2:14][CH2:13][C:12]2[C:15](Cl)=[N:16][C:17]([CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[C:22](Cl)[CH:21]=3)=[N:18][C:11]=2[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:28][O-:29].[Na+]>CO>[CH2:19]([C:17]1[N:16]=[C:15]([O:29][CH3:28])[C:12]2[CH2:13][CH2:14][N:8]([CH2:1][C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)[CH2:9][CH2:10][C:11]=2[N:18]=1)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1

참가 물질

4

반응물 2

HCID 10942334Sodium MethoxideHCID 59312360HCID 59312360, 화합물

생성물 1

HCID 59312304HCID 59312304, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

2,7-dibenzyl-4-chloro-6,7,8,9-tetrahydro-5H-pyrimido[4,5-d]azepine of Step B (86 mg, 0.23 mmol) was dissolved in methanol (10 ml) and sodium methoxide (25 mg, 0.47 mmol) was added. The reaction was refluxed under nitrogen for 16 h. The reaction mixture was concentrated in vacuo and the residue was partitioned between ethyl acetate (50 ml) and water (50 ml). The organic layer was separated, washed with brine (50 ml), dried over MgSO4, filtered and concentrated in vacuo to afford a colourless oil, 75.5 mg, 89%.

후처리

  1. temperatureThe reaction was refluxed under nitrogen for 16 h
  2. concentrationThe reaction mixture was concentrated in vacuo
  3. customthe residue was partitioned between ethyl acetate (50 ml) and water (50 ml)
  4. customThe organic layer was separated
  5. washwashed with brine (50 ml)
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customto afford a colourless oil, 75.5 mg, 89%

출처 및 근거

ORD 기록
ord-528e709b92fa40db876b3c1cd229d716
출처 데이터셋
uspto-grants-2011_04
특허 번호
US07928099B2

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