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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
ノート
印刷プレビュー

反応式

HRID 607152 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
100 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-4119f3aea182472485acdac3d5f669be
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07915411B2

反応ノート

読み込み中…

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