Ethyl Acetate → HCID 86608383、化合物

HRID 641177ノート

反応式

HRID 641177 の反応式
[NH:1]([C:3]1[N:8]=[C:7]([N:9]2[CH2:14][CH2:13][O:12][CH2:11][CH2:10]2)[N:6]=[C:5]([O:15][CH2:16][C:17]([CH3:20])([OH:19])[CH3:18])[CH:4]=1)[NH2:2].[N:21]([O-])=O.[Na+].C(OCC)(=O)C>C(O)(=O)C.O>[N:1]([C:3]1[N:8]=[C:7]([N:9]2[CH2:14][CH2:13][O:12][CH2:11][CH2:10]2)[N:6]=[C:5]([O:15][CH2:16][C:17]([CH3:20])([OH:19])[CH3:18])[CH:4]=1)=[N+:2]=[N-:21]

参加物

6

反応物 3

HCID 8857Ethyl AcetateHCID 23668193Sodium NitriteHCID 68514795HCID 68514795、化合物

生成物 1

HCID 86608383HCID 86608383、化合物

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒

実験手順

1-(6-hydrazino-2-morpholin-4-yl-pyrimidin-4-yloxy)-2-methyl-propan-2-ol was dissolved in glacial acetic acid (30 mL). To this solution was added a solution of sodium nitrite (700 mg) in water (4 mL). The reaction was stirred for ten minutes, and poured into ethyl acetate (100 mL). The organic layer was then washed with water (100 mL) and 10% sodium carbonate (2×100 mL). The organic layer was dried over magnesium sulfate and evaporated to give 1-(6-Azido-2-morpholin-4-yl-pyrimidin-4-yloxy)-2-methyl-propan-2-ol, which was used without purification in the next reaction.

後処理

  1. washThe organic layer was then washed with water (100 mL) and 10% sodium carbonate (2×100 mL)
  2. dry with materialThe organic layer was dried over magnesium sulfate
  3. customevaporated

出典と根拠

ORDレコード
ord-f52c0ab15ece449fbd7058fc9f90a701
出典データセット
uspto-grants-2010_04
特許番号
US07696202B2

反応ノート

読み込み中…