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

HRID 911922

반응식

HRID 911922 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-798b7dc8904d4ced8a8b7b489eb2b41a
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08022223B2

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