2-(2-Bromoethyl)-1,3-dioxolane → Ammonium Hydroxide

HRID 78475

反応式

HRID 78475 の反応式
[NH2:1][C:2]1[S:3][C:4]([CH3:7])=[CH:5][N:6]=1.Br[CH2:9][CH2:10][CH:11]1[O:15][CH2:14][CH2:13][O:12]1>>[NH4+:1].[OH-:12].[O:12]1[CH2:13][CH2:14][O:15][CH:11]1[CH2:10][CH2:9][N:6]1[CH:5]=[C:4]([CH3:7])[S:3][C:2]1=[NH:1]

参加物

4

反応物 2

HCID 877762-(2-Bromoethyl)-1,3-dioxolaneHCID 3517702-Amino-5-methylthiazole

生成物 2

HCID 14923Ammonium HydroxideHCID 686224003-(2-(1,3-dioxolan-2-yl)ethyl)-5-methylthiazol-2(3H)-imine

反応条件

温度
85 °C

実験手順

A mixture of 2-amino-5-methylthiazole (1.0 g, 8.7 mmol) and 2-(2-bromoethyl)-1,3-dioxolane (1.1 mL, 8.7 mmol) was warmed to 85° C. and was allowed to stir for 18 hours. The mixture was cooled to ambient temperature and purified via 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 215 (M+H)+.

後処理

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

出典と根拠

ORDレコード
ord-5c53d03dd8614952b188228f43961fdb
出典データセット
uspto-grants-2014_09
特許番号
US08841334B2

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