Dimethyl Sulfate → 3,5-Dimethyl-2-hydroxymethyl-4-(2,2,3,3,3-pentafluoropropoxy)pyridine

HRID 1248975ノート

反応式

HRID 1248975 の反応式
[CH3:1][C:2]1[CH:3]=[N+:4]([O-])[CH:5]=[C:6]([CH3:17])[C:7]=1[O:8][CH2:9][C:10]([F:16])([F:15])[C:11]([F:14])([F:13])[F:12].S(OC)([O:22][CH3:23])(=O)=O.S(OOS([O-])(=O)=O)([O-])(=O)=O.[NH4+].[NH4+]>O.CO>[CH3:1][C:2]1[C:3]([CH2:23][OH:22])=[N:4][CH:5]=[C:6]([CH3:17])[C:7]=1[O:8][CH2:9][C:10]([F:16])([F:15])[C:11]([F:14])([F:13])[F:12]

参加物

6

反応物 3

HCID 6497Dimethyl SulfateHCID 62648Ammonium PersulfateHCID 136548073,5-Dimethyl-4-(2,2,3,3,3-pentafluoropropoxy)pyridine-1-oxide

生成物 1

HCID 149020163,5-Dimethyl-2-hydroxymethyl-4-(2,2,3,3,3-pentafluoropropoxy)pyridine

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 962Water溶媒

反応条件

温度
120 °C

実験手順

A mixture of 3,5-dimethyl-4-(2,2,3,3,3-pentafluoropropoxy)pyridine-1-oxide (2.5 g) and dimethyl sulfate (1 ml) was heated at 120° C. for 30 minutes, to which was then added methanol (12.5 ml). To the mixture was added dropwise at 80° C. ammonium persulfate (4.3 g) dissolved in water (20 ml)-methanol (10 ml) over 30 minutes, which was stirred for further 30 minutes. The resultant solution was concentrated. To the residue was added ice, which was neutralized with sodium carbonate, followed by extraction with chloroform. The extract was dried on sodium sulfate, followed by removing the solvent by evaporation to give 2.2 g of 3,5-dimethyl-2-hydroxymethyl-4-(2,2,3,3,3-pentafluoropropoxy)pyridine as an oily substance.

後処理

  1. concentrationThe resultant solution was concentrated
  2. additionTo the residue was added ice, which
  3. extractionfollowed by extraction with chloroform
  4. customThe extract was dried on sodium sulfate
  5. customby removing the solvent
  6. customby evaporation

出典と根拠

ORDレコード
ord-b54aad2f10484b4dada1613305783923
出典データセット
uspto-grants-1986_12
特許番号
US04628098

反応ノート

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