Hexane → HCID 14458736、化合物

HRID 1651035ノート

反応式

HRID 1651035 の反応式
Cl.[C:2]1([CH3:18])[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[O:8][C:9]1[N:14]=[C:13]([C:15]([NH2:17])=[NH:16])[CH:12]=[CH:11][CH:10]=1.C[O-].[Na+].[CH3:22][CH2:23][CH2:24][CH2:25]CC.C(OCC)(=O)C>CO.COC(OC)C(=O)CC>[CH3:25][C:24]1[CH:23]=[CH:22][N:17]=[C:15]([C:13]2[CH:12]=[CH:11][CH:10]=[C:9]([O:8][C:3]3[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=3[CH3:18])[N:14]=2)[N:16]=1

参加物

7

反応物 4

HCID 8058HexaneHCID 8857Ethyl AcetateHCID 10942334Sodium MethoxideHCID 23051377HCID 23051377、化合物

生成物 1

HCID 14458736HCID 14458736、化合物収率 76%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 2420211,1-dimethoxybutan-2-one溶媒

実験手順

To a mixture of 6-o-tolyloxy-2-picoline amidine hydrochloride (3 g) and methanol (100 ml) were added 28% sodium methoxide solution in methanol (3.3 g) and 1,1-dimethoxybutanone (1.9 g). The mixture was heated under refluxing for an hour, and was left to stand at room temperature. The reaction solution was concentrated under reduced pressure, and the residue obtained was subjected to silica gel column chromatography (eluent; n-hexane: ethyl acetate=2:1 in volume) to obtain 4-methyl-2-(6-o-tolyloxy-2-pyridinyl)pyrimidine (2.4 g, yield 76%).

後処理

  1. temperatureThe mixture was heated
  2. temperatureunder refluxing for an hour
  3. waitwas left
  4. customto stand at room temperature
  5. concentrationThe reaction solution was concentrated under reduced pressure
  6. customthe residue obtained

出典と根拠

ORDレコード
ord-b8b47f47bd9b492ebf1058464026954d
出典データセット
uspto-grants-1990_05
特許番号
US04927827

反応ノート

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