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Hydrochloric Acid → (E)-3-(3,3-Dimethyl-2-oxo-2,3,4,5-tetrahydro-1H-pyrido[2,3-e][1,4]diazepin-7-yl)-N-(3-isopropyl-2-propoxybenzyl)-N-methylacrylamide hydrochloride

HRID 2097038
ノート
印刷プレビュー

反応式

HRID 2097038 の反応式
[CH3:1][C:2]1([CH3:34])[C:8](=[O:9])[NH:7][C:6]2[N:10]=[CH:11][C:12](/[CH:14]=[CH:15]/[C:16]([N:18]([CH2:20][C:21]3[CH:26]=[CH:25][CH:24]=[C:23]([CH:27]([CH3:29])[CH3:28])[C:22]=3[O:30][CH2:31][CH2:32][CH3:33])[CH3:19])=[O:17])=[CH:13][C:5]=2[CH2:4][NH:3]1.[ClH:35]>C(Cl)Cl.C(OCC)C>[ClH:35].[CH3:34][C:2]1([CH3:1])[C:8](=[O:9])[NH:7][C:6]2[N:10]=[CH:11][C:12](/[CH:14]=[CH:15]/[C:16]([N:18]([CH2:20][C:21]3[CH:26]=[CH:25][CH:24]=[C:23]([CH:27]([CH3:29])[CH3:28])[C:22]=3[O:30][CH2:31][CH2:32][CH3:33])[CH3:19])=[O:17])=[CH:13][C:5]=2[CH2:4][NH:3]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 16659657(E)-3-(3,3-Dimethyl-2-oxo-2,3,4,5-tetrahydro-1H-pyrido[2,3-e][1,4]diazepin-7-yl)-N-(3-isopropyl-2-propoxybenzyl)-N-methylacrylamide

生成物 1

HCID 16659656(E)-3-(3,3-Dimethyl-2-oxo-2,3,4,5-tetrahydro-1H-pyrido[2,3-e][1,4]diazepin-7-yl)-N-(3-isopropyl-2-propoxybenzyl)-N-methylacrylamide hydrochloride収率 71%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒
HCID 6344
Dichloromethane
溶媒

実験手順

A stirring solution of (E)-3-(3,3-dimethyl-2-oxo-2,3,4,5-tetrahydro-1H-pyrido[2,3-e][1,4]diazepin-7-yl)-N-(3-isopropyl-2-propoxybenzyl)-N-methylacrylamide (0.164 g, 0.352 mmol) in CH2Cl2 (4 mL) under N2 was treated with anhydrous HCl (0.17 mL of a 2.0 M solution in diethyl ether, 0.34 mmol) After stirring for 18 h, the resulting solid was collected by filtration, washed with Et2O (100 mL) and dried to yield the title compound (0.12 g, 71%) as an off white solid and as a mixture of amide rotamers: 1H NMR (300 MHz, DMSO-d6) δ 10.95 (br s, 1H), 10.25 (br s, 2H), 8.67-8.63 (m, 1H), 8.36-8.26 (m, 1H), 7.62-7.54 (m, 1H), 7.39-7.31 (m, 1H), 7.26-7.20 (m, 1H), 7.13-7.05 (m, 1H), 6.90-6.84 (m, 1H), 4.82-4.67 (m, 2H), 4.41-4.36 (m, 2H), 3.77-3.69 (m, 2H), 3.30-3.25 (m, 1H), 3.16-2.89 (m, 3H), 1.82-1.75 (m, 2H), 1.60-1.58 (m, 6H), 1.23-1.13 (m, 6H), 1.06-1.01 (m, 3H); MS (ESI) m/e 465 (M+H)+.

後処理

  1. filtrationthe resulting solid was collected by filtration
  2. washwashed with Et2O (100 mL)
  3. customdried

出典と根拠

ORDレコード
ord-7644b9299d9448a7831ac88404cc1c90
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08450307B2

反応ノート

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