Methyl chloroformate → Methyl [6-(trifluoromethyl)pyridin-3-yl]carbamate
反応式
[F:1][C:2]([F:11])([F:10])[C:3]1[N:8]=[CH:7][C:6]([NH2:9])=[CH:5][CH:4]=1.Cl[C:13]([O:15][CH3:16])=[O:14].C(=O)(O)[O-].[Na+]>N1C=CC=CC=1>[F:11][C:2]([F:1])([F:10])[C:3]1[N:8]=[CH:7][C:6]([NH:9][C:13](=[O:14])[O:15][CH3:16])=[CH:5][CH:4]=1参加物
5
実験手順
Into 15 ml of pyridine was dissolved 3.00 g of 6-(trifluoromethyl)pyridin-3-amine, and then 2.1 ml of methyl chloroformate was added thereto under ice-cooling, followed by 2 hours of stirring at room temperature. Under ice-cooling, 30 ml of a saturated sodium bicarbonate aqueous solution was added to the reaction solution, followed by 1 hour of stirring. Thereafter, the precipitated crystals were filtrated and, after washing with water, dried under reduced pressure to obtain 3.88 g of the title compound.
後処理
- temperatureunder ice-cooling
- temperatureUnder ice-cooling
- waitfollowed by 1 hour
- stirringof stirring
- filtrationThereafter, the precipitated crystals were filtrated
- washafter washing with water
- customdried under reduced pressure
出典と根拠
- ORDレコード
- ord-5559a5419f414fab9b82dd2c322ea1b0
- 出典データセット
- uspto-grants-2007_11
- 特許番号
- US07297698B2
反応ノート
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