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2,2-Dimethyl-1,3-dioxane-4,6-dione → 2,2-Dimethyl-5-[(1-methyl-1H-pyrazol-3-ylamino)-methylene]-[1,3]dioxane-4,6-dione

HRID 607152
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인쇄 미리보기

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HRID 607152 반응식
[CH3:1][N:2]1[CH:6]=[CH:5][C:4]([NH2:7])=[N:3]1.[CH3:8][C:9]1([CH3:17])[O:14][C:13](=[O:15])[CH2:12][C:11](=[O:16])[O:10]1.[CH2:18](OC(OCC)OCC)C>CCO>[CH3:8][C:9]1([CH3:17])[O:14][C:13](=[O:15])[C:12](=[CH:18][NH:7][C:4]2[CH:5]=[CH:6][N:2]([CH3:1])[N:3]=2)[C:11](=[O:16])[O:10]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 162492,2-Dimethyl-1,3-dioxane-4,6-dioneHCID 31214Ethyl orthoformateHCID 1372541-Methyl-3-aminopyrazole

생성물 1

HCID 670477842,2-Dimethyl-5-[(1-methyl-1H-pyrazol-3-ylamino)-methylene]-[1,3]dioxane-4,6-dione수율 66.7%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
100 °C

실험 절차

A mixture of 1-methyl-1H-pyrazol-3-ylamine (1.05 g, 10.8 mmol), 2,2-dimethyl-[1,3]dioxane-4,6-dione (1.71 g, 11.9 mmol), and triethylorthoformate (1.60 g, 10.8 mmol,) in a 25 mL round bottomed flask was heated in a 100° C. oil bath for 15 min. The mixture was cooled to room temperature and EtOH (10 mL) was added. The reaction mixture was heated to dissolve all solids and then cooled back to room temperature. The solid that was formed was isolated by filtration, rinsed with ethanol, and dried to provide the title compound (1.81 g, 66% yield).

후처리

  1. temperatureThe mixture was cooled to room temperature
  2. temperatureThe reaction mixture was heated
  3. dissolutionto dissolve all solids
  4. temperaturecooled back to room temperature
  5. customThe solid that was formed
  6. customwas isolated by filtration
  7. washrinsed with ethanol
  8. customdried

출처 및 근거

ORD 기록
ord-4119f3aea182472485acdac3d5f669be
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07915411B2

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