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

HRID 1923482ノート

反応式

HRID 1923482 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-85ab660f24094748a431a01a41def725
出典データセット
uspto-grants-2012_05
特許番号
US08178526B2

反応ノート

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