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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-methyl-N-(2-propoxy-3-trifluoromethoxybenzyl)acrylamide hydrochloride

HRID 1362267
ノート
印刷プレビュー

反応式

HRID 1362267 の反応式
[CH3:1][C:2]1([CH3:36])[C:8](=[O:9])[NH:7][C:6]2[N:10]=[CH:11][C:12](/[CH:14]=[CH:15]/[C:16]([N:18]([CH3:35])[CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[C:22]([O:26][C:27]([F:30])([F:29])[F:28])[C:21]=3[O:31][CH2:32][CH2:33][CH3:34])=[O:17])=[CH:13][C:5]=2[CH2:4][NH:3]1.[ClH:37]>C(Cl)Cl.C(OCC)C>[ClH:37].[CH3:36][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]([CH3:35])[CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[C:22]([O:26][C:27]([F:29])([F:30])[F:28])[C:21]=3[O:31][CH2:32][CH2:33][CH3:34])=[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 16662046HCID 16662046、化合物

生成物 1

HCID 16662045(E)-3-(3,3-Dimethyl-2-oxo-2,3,4,5-tetrahydro-1H-pyrido[2,3-e][1,4]diazepin-7-yl)-N-methyl-N-(2-propoxy-3-trifluoromethoxybenzyl)acrylamide hydrochloride収率 82%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6344Dichloromethane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-methyl-N-(2-propoxy-3-trifluoromethoxybenzyl)acrylamide (0.255 g, 0.503 mmol) in CH2Cl2 (5 mL) under N2, was treated with anhydrous HCl (0.25 mL of a 2 M solution in diethyl ether, 0.5 mmol). After stirring for 18 h, the resulting solid was collected by filtration and washed with Et2O (150 mL). The solid was dried under vacuum to yield the target compound (0.21 g, 82%) as an off white solid and as a mixture of amide rotamers: 1H NMR (300 MHz, DMSO-d6) δ 10.93-10.91 (m, 1H), 10.51 (br s, 2H), 8.66-8.64 (m, 1H), 8.40-8.32 (m, 1H), 7.63-7.54 (m, 1H), 7.40-7.09 (m, 4H), 4.89-4.70 (m, 2H), 4.41-4.36 (m, 2H), 3.96-3.90 (m, 2H), 3.18-2.87 (m, 3H), 1.79-1.70 (m, 2H), 1.63-1.61 (m, 6H), 1.09-0.97 (m, 3H); MS (ESI) m/e 507 (M+H)+.

後処理

  1. filtrationthe resulting solid was collected by filtration
  2. washwashed with Et2O (150 mL)
  3. customThe solid was dried under vacuum

出典と根拠

ORDレコード
ord-c7125a1f43a7465a9438b7493287928e
出典データセット
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07879872B2

反応ノート

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