Hydrochloric Acid → HCID 57448161、化合物
反応式
[CH:1]1([S:4][C:5]2[CH:12]=[CH:11][CH:10]=[CH:9][C:6]=2[C:7]#[N:8])[CH2:3][CH2:2]1.S(C)C.[ClH:16]>C1COCC1>[ClH:16].[CH:1]1([S:4][C:5]2[CH:12]=[CH:11][CH:10]=[CH:9][C:6]=2[CH2:7][NH2:8])[CH2:3][CH2:2]1参加物
5
実験手順
To 1A (1.50 g, 7.25 mmol) in refluxing THF (72 mL) was added a 2M THF solution of BH3.SMe2 (10.8 mL, 21.7 mmol). After heating at reflux for 2 h, the reaction was cooled to rt and 6M HCl (4.32 mL) was slowly added. The reaction was heated to reflux for 30 min, then cooled to rt, concentrated and azeotroped (3×) with THF/MeOH on a rotary evaporator. The resulting residue was taken up in THF and filtered to provide 1B (1.40 g, 79%) as a white solid. 1H NMR (400 MHz, CD3OD) δ ppm 1.15 (m, 2H) 1.29 (m, 2H) 2.91 (m, 1H) 4.52 (s, 2H) 7.72 (m, J=7.69, 7.69 Hz, 2H) 7.80 (t, J=6.81 Hz, 1H) 8.04 (d, J=7.91 Hz, 1H).
後処理
- temperatureAfter heating
- temperatureat reflux for 2 h
- temperatureThe reaction was heated
- temperatureto reflux for 30 min
- temperaturecooled to rt
- concentrationconcentrated
- customazeotroped (3×) with THF/MeOH
- customon a rotary evaporator
- filtrationfiltered
出典と根拠
- ORDレコード
- ord-98c0fe9cac714b6d91868400869e3df4
- 出典データセット
- uspto-grants-2011_10
- 特許番号
- US08044242B2
反応ノート
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