Butyl iodide → 4,6-Dibutoxy-2-trifluoromethylpyridine-3-carboxylic acid ethyl ester

HRID 1251950노트

반응식

HRID 1251950 반응식
[OH:1][C:2]1[CH:7]=[C:6]([OH:8])[N:5]=[C:4]([C:9]([F:12])([F:11])[F:10])[C:3]=1[C:13]([O:15][CH2:16][CH3:17])=[O:14].[CH2:18](I)[CH2:19][CH2:20][CH3:21].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH2:18]([O:1][C:2]1[CH:7]=[C:6]([O:8][CH2:7][CH2:2][CH2:3][CH3:4])[N:5]=[C:4]([C:9]([F:12])([F:10])[F:11])[C:3]=1[C:13]([O:15][CH2:16][CH3:17])=[O:14])[CH2:19][CH2:20][CH3:21]

참가 물질

5

반응물 3

HCID 10962Butyl iodideHCID 11430Potassium CarbonateHCID 178470040HCID 178470040, 화합물

생성물 1

HCID 137267874,6-Dibutoxy-2-trifluoromethylpyridine-3-carboxylic acid ethyl ester수율 198.8%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mechanically stirred mixture of 22.6 g (0.09 mol) of product of Example 1, 99 g of butyl iodide, 24.84 g of potassium carbonate and 250 ml of acetone was held at reflux for 26 hours and filtered. The acetone filtrate was concentrated and the residue was dissolved in ether. The ether solution was washed with water, dried, and concentrated. The residue was kugelrohr distilled at 0.3 torr to give 32.5 g (99%) of product, nD25 1.4543.

후처리

  1. temperatureat reflux for 26 hours
  2. filtrationfiltered
  3. concentrationThe acetone filtrate was concentrated
  4. dissolutionthe residue was dissolved in ether
  5. washThe ether solution was washed with water
  6. customdried
  7. concentrationconcentrated
  8. distillationThe residue was kugelrohr distilled at 0.3 torr

출처 및 근거

ORD 기록
ord-becb1e6e299d4f4dacf779ec6e58188c
출처 데이터셋
uspto-grants-1988_05
특허 번호
US04741766

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