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

HRID 622158노트

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HRID 622158 반응식
[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.CO.S(OOS([O-])(=O)=O)([O-])(=O)=O.[NH4+].[NH4+]>O>[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]

참가 물질

6

반응물 4

HCID 887Methanol2회HCID 6497Dimethyl SulfateHCID 62648Ammonium PersulfateHCID 136548073,5-Dimethyl-4-(2,2,3,3,3-pentafluoropropoxy)pyridine-1-oxide

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

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온도
120 °C

실험 절차

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 and methanol (12.5 ml) was added, after which a solution of ammonium persulfate (4.3 g) in water (20 ml)-methanol (10 ml) was added dropwise at 80° C. over a period of 30 minutes and the mixture was stirred for 30 minutes. After concentration, ice was added and the mixture was neutralized with sodium carbonate, and then was extracted with chloroform. After drying the extract over sodium sulfate, the solvent was evaporated to give 2.2 g of 3,5-dimethyl-2-hydroxymethyl-4-(2,2,3,3,3pentafluoropropoxy)pyridine as oil.

후처리

  1. concentrationAfter concentration, ice
  2. additionwas added
  3. extractionwas extracted with chloroform
  4. customAfter drying the
  5. extractionextract over sodium sulfate
  6. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-2470191b9cc84d31a7bb1d8528010a67
출처 데이터셋
uspto-grants-1988_09
특허 번호
US04769456

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