Trimethyl orthoformate → 2,2-Dimethyl-5-((4-methylthiophen-3-ylamino)methylene)-1,3-dioxane-4,6-dione

HRID 335245

反応式

HRID 335245 の反応式
[CH3:1][C:2]1([CH3:10])[O:7][C:6](=[O:8])[CH2:5][C:4](=[O:9])[O:3]1.[CH3:11]OC(OC)OC.[CH3:18][C:19]1[C:20]([NH2:24])=[CH:21][S:22][CH:23]=1>>[CH3:1][C:2]1([CH3:10])[O:7][C:6](=[O:8])[C:5](=[CH:11][NH:24][C:20]2[C:19]([CH3:18])=[CH:23][S:22][CH:21]=2)[C:4](=[O:9])[O:3]1

参加物

4

反応物 3

HCID 9005Trimethyl orthoformate2 回HCID 162492,2-Dimethyl-1,3-dioxane-4,6-dioneHCID 57433964-Methylthiophen-3-amine

生成物 1

HCID 669953662,2-Dimethyl-5-((4-methylthiophen-3-ylamino)methylene)-1,3-dioxane-4,6-dione収率 99%

反応条件

温度
90 °C

実験手順

A stirred solution of 2,2-dimethyl-1,3-dioxane-4,6-dione (4.85 g, 34 mmol) in trimethoxymethane (37 mL, 337 mmol) was heated to 90° C. under nitrogen. After 2 hours, a solution was 4-methylthiophen-3-amine (3.81 g, 34 mmol) was added (as a solution in trimethoxymethane (37 mL, 337 mmol). The reaction stirred at 90° C. for 6 hours and then was allowed to cool to room temperature and concentrated. The material was placed in the refrigerator where it solidified after two days to obtain the title compound (9 g, quantitative).

後処理

  1. temperatureto cool to room temperature
  2. concentrationconcentrated
  3. waitsolidified after two days

出典と根拠

ORDレコード
ord-6e74fe5b0aed42ee8b902148a42c9844
出典データセット
uspto-grants-2014_11
特許番号
US08883828B2

関連ノート

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