Dimethylformamide → HCID 19096639、化合物

HRID 1657201ノート

反応式

HRID 1657201 の反応式
[N-:1]=[N+:2]=[N-:3].[Na+].CN(C=O)C.[CH3:10][C:11]1([CH3:23])[O:16][C:15](=[O:17])[CH:14]=[C:13]([CH2:18][C:19](=[O:22])[CH2:20]Cl)[O:12]1>C(OCC)(=O)C>[CH3:10][C:11]1([CH3:23])[O:16][C:15](=[O:17])[CH:14]=[C:13]([CH2:18][C:19](=[O:22])[CH2:20][N:1]=[N+:2]=[N-:3])[O:12]1

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 33557Sodium AzideHCID 149448286-(3-Chloro-2-oxopropyl)-2,2-dimethyl-2H,4H-1,3-dioxin-4-one

生成物 1

HCID 19096639HCID 19096639、化合物収率 82.3%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

195 mg (3.0 mmol) of sodium azide were added to 2 ml of a DMF solution containing 328 mg (1.5 mmol) of 2,2-dimethyl-6-(3-chloro-2-oxopropyl)-1,3-dioxin-4-one prepared in Example 1, followed by stirring at room temperature for 10 minutes. Afterward, the solution was poured into ice water, extracted with ether, and then dried with anhydrous magnesium sulfate. After ether was distilled off, the residue was then subjected to column chromatography (an eluent of hexane:ethyl acetate=1:1), thereby obtaining 278 mg (yield 82%) of 2,2-dimethyl-6-(3-azido-2-oxopropyl)-1,3-dioxin-4-one.

後処理

  1. extractionextracted with ether
  2. dry with materialdried with anhydrous magnesium sulfate
  3. distillationAfter ether was distilled off

出典と根拠

ORDレコード
ord-28c6f3cbbc37419ba606fc6727ae7467
出典データセット
uspto-grants-1993_10
特許番号
US05256800

反応ノート

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