2,4-Dichlorobenzoyl chloride → HCID 69351048、化合物

反応式

[Cl:1][C:2]1[CH:10]=[C:9]([Cl:11])[CH:8]=[CH:7][C:3]=1[C:4](Cl)=[O:5].[CH3:12][N:13]([CH3:27])[CH:14]1[CH2:19][CH2:18][C:17]([C:20]2[N:25]=[C:24]([NH2:26])[CH:23]=[CH:22][CH:21]=2)=[CH:16][CH2:15]1>>[ClH:1].[ClH:1].[Cl:1][C:2]1[CH:10]=[C:9]([Cl:11])[CH:8]=[CH:7][C:3]=1[C:4]([NH:26][C:24]1[CH:23]=[CH:22][CH:21]=[C:20]([C:17]2[CH2:18][CH2:19][CH:14]([N:13]([CH3:27])[CH3:12])[CH2:15][CH:16]=2)[N:25]=1)=[O:5]

参加物

反応物 2

HCID 666452,4-Dichlorobenzoyl chloride

HCID 588523656-(4-Dimethylamino-cyclohex-1-enyl)-pyridin-2-ylamine

生成物 1

HCID 69351048HCID 69351048、化合物収率 67%

実験手順

Using a method similar to example 1, using 2,4-dichloro-benzoyl chloride (126 mg, 0.60 mmol) and 6-(4-dimethylamino-cyclohex-1-enyl)-pyridin-2-ylamine, isomer 1 (preparation 10, 100 mg, 0.46 mmol) provides the free base of the title compound as a colorless oil (120 mg, 67%): MS (ES): m/z=390.1 (M+H)+; 1H NMR (CDCl3): δ 8.90 (s, br, 1H), 8.20 (d, 1H), 7.73 (t, 1H), 7.57 (d, 1H), 7.45 (d, 1H), 7.28 (dd, 1H), 7.14 (d, 1H), 6.63 (m, 1H), 2.67 (m, 1H), 2.44 (m, 3H), 2.36 (s, 6H), 2.15 (m, 2H), 1.54 (m, 1H). Di-hydrochloride salt: Anal. cal'd for C20H21Cl2N3O.2HCl: C, 51.86; H, 5.00; N, 9.07. Found: C, 51.78; H, 5.04; N, 8.99.

出典と根拠

ORDレコード: ord-4b913f7df46f4f50904f98e453e96fc2
出典データセット: uspto-grants-2007_12
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US07312236B2

反応ノート

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