2-(Bromomethyl)tetrahydro-2H-pyran → Ammonia

HRID 255119

反応式

HRID 255119 の反応式
[NH2:1][C:2]1[S:3][C:4]([CH3:7])=[CH:5][N:6]=1.Br[CH2:9][CH:10]1[CH2:15][CH2:14][CH2:13][CH2:12][O:11]1>>[NH4+:1].[OH-:11].[CH3:7][C:4]1[S:3][C:2](=[NH:1])[N:6]([CH2:9][CH:10]2[CH2:15][CH2:14][CH2:13][CH2:12][O:11]2)[CH:5]=1.[NH3:1]

参加物

5

反応物 2

HCID 1419172-(Bromomethyl)tetrahydro-2H-pyranHCID 3517702-Amino-5-methylthiazole

生成物 3

HCID 222AmmoniaHCID 14923Ammonium HydroxideHCID 668596105-Methyl-3-(tetrahydro-pyran-2-ylmethyl)-3H-thiazol-2-ylideneamine

反応条件

温度
85 °C

実験手順

A mixture of 2-amino-5-methylthiazole (1.2 g, 11 mmol) and 2-(bromomethyl)tetrahydro-2H-pyran (1.5 mL, 12 mmol) was warmed to 85° C. and stirred for 18 hours. The mixture was cooled to ambient temperature and purified via flash column chromatography (SiO2, 10% methanol in ethyl acetate then 9:1:0.1 CH2Cl2:methanol:NH4OH) to afford the title compound MS (DCI/NH3) m/z 213 (M+H)+.

後処理

  1. temperatureThe mixture was cooled to ambient temperature
  2. custompurified via flash column chromatography (SiO2, 10% methanol in ethyl acetate

出典と根拠

ORDレコード
ord-364c5e65b6104f5e9e835916c10da7f5
出典データセット
uspto-grants-2011_01
特許番号
US07875639B2

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