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

HRID 335245

반응식

HRID 335245 반응식
[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

참가 물질

4

반응물 3

HCID 9005Trimethyl orthoformate2회HCID 162492,2-Dimethyl-1,3-dioxane-4,6-dioneHCID 57433964-Methylthiophen-3-amine

생성물 1

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

반응 조건

온도
90 °C

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-6e74fe5b0aed42ee8b902148a42c9844
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08883828B2

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