Diisopropylethylamine → 2-Chloro-5-(isocyanatomethyl)thiophene
反応式
Cl[C:2](Cl)([O:4]C(=O)OC(Cl)(Cl)Cl)Cl.[Cl:13][C:14]1[S:18][C:17]([CH2:19][NH2:20])=[CH:16][CH:15]=1.CCN(C(C)C)C(C)C>C(Cl)Cl>[Cl:13][C:14]1[S:18][C:17]([CH2:19][N:20]=[C:2]=[O:4])=[CH:16][CH:15]=1参加物
5
実験手順
To a solution of triphosgene (1.15 g, 3.9 mmol) in CH2Cl2 (30 mL) was added dropwise a mixture of (5-chlorothiophen-2-yl)methanamine (1.14 g, 7.8 mmol) and DIPEA (2.0 g, 15.6 mmol) in CH2Cl2 (32 mL) over 2 hours at 0 C under N2 atmosphere. After addition was complete, the mixture was refluxed for 1 hour and then cooled to ambient temperature. The mixture was washed with aq. KHSO4, brine, dried over Na2SO4, and concentrated to give 5-chlorothiophen-2-yl-methyl isocynate a yellow liquid (1.34 g, yield 100%), which was used in the next step without further purification.
後処理
- additionAfter addition
- temperaturethe mixture was refluxed for 1 hour
- washThe mixture was washed with aq. KHSO4, brine
- dry with materialdried over Na2SO4
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-5b6924ca86554f28a96b602e3ea6eb6b
- 出典データセット
- uspto-grants-2012_04
- 特許番号
- US08148380B2
反応ノート
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