2-Chloropyridine → 1-(PYRIDIN-2-YL)-1,4-DIAZEPANE

HRID 530460ノート

反応式

HRID 530460 の反応式
Cl[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][N:3]=1.CCN(C(C)C)C(C)C.[NH:17]1[CH2:23][CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1>CC(N(C)C)=O>[N:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=1[N:17]1[CH2:23][CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1

参加物

5

反応物 3

HCID 79772-ChloropyridineHCID 68163Hexahydro-1,4-diazepineHCID 81531Diisopropylethylamine

生成物 1

HCID 27724021-(PYRIDIN-2-YL)-1,4-DIAZEPANE収率 72.9%

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

2-Chloropyridine (3.00 g, 26.4 mmol), DIPEA (9.20 mL, 52.8 mmol) and homopiperazine (7.90 g, 79.3 mmol) were dissolved in DMA (10 mL) and heated using a microwave (180-200° C., absorption high) for 40 min. The reaction mixture was diluted with DCM (150 mL), washed with sat aq Na2CO3 (100 mL), brine (100 mL), dried (MgSO4) and concentrated in vacuo to give the title compound (3.41 g, 72%) as a brown liquid. LCMS (ES+): 178.6 [MH]+.

後処理

  1. temperatureheated
  2. customa microwave (180-200° C., absorption high) for 40 min
  3. additionThe reaction mixture was diluted with DCM (150 mL)
  4. washwashed
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-5d2248bae6df4f3cad04ce8548b8b349
出典データセット
uspto-grants-2016_05
特許番号
US09353086B2

反応ノート

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