Sodium Methoxide → HCID 59312304、化合物

HRID 2077057ノート

反応式

HRID 2077057 の反応式
[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

参加物

4

反応物 2

HCID 10942334Sodium MethoxideHCID 59312360HCID 59312360、化合物

生成物 1

HCID 59312304HCID 59312304、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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%.

後処理

  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%

出典と根拠

ORDレコード
ord-528e709b92fa40db876b3c1cd229d716
出典データセット
uspto-grants-2011_04
特許番号
US07928099B2

反応ノート

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