Sodium Hydroxide → 8-chloro-2,3,4,5-tetrahydro-1-methyl-1H-3-benzazepine
反応式
FC(F)(F)C([N:5]1[CH2:11][CH:10]([CH3:12])[C:9]2[CH:13]=[C:14]([Cl:17])[CH:15]=[CH:16][C:8]=2[CH2:7][CH2:6]1)=O.[OH-].[Na+]>CO>[Cl:17][C:14]1[CH:15]=[CH:16][C:8]2[CH2:7][CH2:6][NH:5][CH2:11][CH:10]([CH3:12])[C:9]=2[CH:13]=1参加物
4
実験手順
A solution of N-trifluoroacetyl-8-chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine (65 mg, 0.22 mmol) in methanol (2 mL) was treated with 15% aqueous NaOH (2 mL), and stirred for 3.5 hours at 60 C. The product mixture was concentrated, extracted 3 times with CH2Cl2 (5 mL), dried with Na2SO4 and concentrated to give 35 mg of a clear oil. 1H NMR (400 MHz, CDCl3) d 7.11 (s, 1H), 7.05 (d, J=8 Hz, 1H), 6.98 (d, J=8 Hz, 1H), 3.1-2.9 (m, 6H), 2.71 (m, 1H), 2.68 (bs, 1H), 1.32 (d, J=8 Hz, 3H). MS calculated for C11H14ClN+H: 196, observed: 196.
後処理
- concentrationThe product mixture was concentrated
- extractionextracted 3 times with CH2Cl2 (5 mL)
- dry with materialdried with Na2SO4
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-46898299f0e4455ea298e1628a659789
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08846906B2
反応ノート
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