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

HRID 1806171ノート

反応式

HRID 1806171 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-760de29f7e354ec58c3c4562e94fcb76
出典データセット
uspto-grants-2013_01
特許番号
US08354540B2

反応ノート

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