2,2,2-Trifluoroethanol → HCID 67938850、化合物

HRID 622705ノート

反応式

HRID 622705 の反応式
[F:1][C:2]([F:6])([F:5])[CH2:3][OH:4].[H-].[Na+].[Na].Br[C:11]1[CH:16]=[CH:15][C:14]([CH2:17][N:18]2[CH2:22][CH2:21][NH:20][C:19]2=[CH:23][N+:24]([O-:26])=[O:25])=[CH:13][N:12]=1>C1(C)C=CC=CC=1>[F:1][C:2]([F:6])([F:5])[CH2:3][O:4][C:11]1[CH:16]=[CH:15][C:14]([CH2:17][N:18]2[CH2:22][CH2:21][NH:20][C:19]2=[CH:23][N+:24]([O-:26])=[O:25])=[CH:13][N:12]=1

参加物

6

反応物 4

HCID 64092,2,2-Trifluoroethanol2 回HCID 24758Sodium hydrideHCID 5360545SodiumHCID 85528837HCID 85528837、化合物

生成物 1

HCID 67938850HCID 67938850、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
80 °C

実験手順

2,2,2-Trifluoroethanol (3.6 g) was dissolved in toluene (20 ml), and sodium hydride (0.7 g) was added to prepare a sodium salt of 2,2,2-trifluoroethanol. Then, 3 g of 1-(2-bromo-5-pyridylmethyl)-2-(nitromethylene)imidazolidine (the known compound described in Japanese Patent Application No. 132,943/1984) was added, and the mixture was heated at 80° C. for 8 hours. Toluene was distilled off under reduced pressure, and the residue was poured into 20 ml of ice water and then neutralized. The aqueous solution was extracted with dichloromethane, and the extract was purified by silica gel column chromatography to give 1-[2-(2,2,2-trifluoroethoxy)-5-pyridylmethyl]-2-(nitromethylene)-imidazolidine. mp. 132°-135° C.

後処理

  1. addition132,943/1984) was added
  2. distillationToluene was distilled off under reduced pressure
  3. additionthe residue was poured into 20 ml of ice water
  4. extractionThe aqueous solution was extracted with dichloromethane
  5. customthe extract was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-f16100821cc943d5b3100d9fffe02296
出典データセット
uspto-grants-1988_09
特許番号
US04772620

反応ノート

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