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

HRID 1251950ノート

反応式

HRID 1251950 の反応式
[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]

参加物

5

反応物 3

HCID 10962Butyl iodideHCID 11430Potassium CarbonateHCID 178470040HCID 178470040、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-becb1e6e299d4f4dacf779ec6e58188c
出典データセット
uspto-grants-1988_05
特許番号
US04741766

反応ノート

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