Hexahydro-1,4-diazepine → 1-[5-(Trifluoromethyl)pyridin-2-yl]-1,4-diazepane

HRID 1923482노트

반응식

HRID 1923482 반응식
Cl[C:2]1[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][N:3]=1.[NH:12]1[CH2:18][CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1>CN(C=O)C>[F:9][C:8]([F:11])([F:10])[C:5]1[CH:6]=[CH:7][C:2]([N:12]2[CH2:18][CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)=[N:3][CH:4]=1

참가 물질

4

반응물 2

HCID 68163Hexahydro-1,4-diazepineHCID 923422-Chloro-5-(trifluoromethyl)pyridine

생성물 1

HCID 27607791-[5-(Trifluoromethyl)pyridin-2-yl]-1,4-diazepane

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 2-chloro-5-trifluoromethylpyridine (362 mg, 1.99 mmol) and [1,4]-diazepane (1000 mg, 9.98 mmol) in DMF (6.0 mL) is stirred for 2 hours at room temperature followed by evaporation of the solvent DMF under vacuo. The residue is distributed between ethyl acetate (30 mL) and water (40 mL). The aqueous phase is extracted once with ethyl acetate (20 m) and the combined organic phases are dried with Na2SO4. Evaporation gives an oily residue (crude 1-(5-trifluoromethyl-pyridin-2-yl)-[1,4]-diazepane) which is used directly for reductive amination in the last step.

후처리

  1. customfollowed by evaporation of the solvent DMF under vacuo
  2. extractionThe aqueous phase is extracted once with ethyl acetate (20 m)
  3. dry with materialthe combined organic phases are dried with Na2SO4
  4. customEvaporation

출처 및 근거

ORD 기록
ord-85ab660f24094748a431a01a41def725
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08178526B2

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