2,2,2-Trifluoroethanol → HCID 67938850, 화합물

HRID 1193960노트

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HRID 1193960 반응식
[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

참가 물질

6

반응물 4

HCID 64092,2,2-Trifluoroethanol2회HCID 24758Sodium hydrideHCID 5360545SodiumHCID 85528837HCID 85528837, 화합물

생성물 1

HCID 67938850HCID 67938850, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-eab6d073de5446bcb02a9879713e7010
출처 데이터셋
uspto-grants-1989_03
특허 번호
US04812454

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