Dimethylformamide → HCID 19096639, 화합물

HRID 1657201노트

반응식

HRID 1657201 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 19096639HCID 19096639, 화합물수율 82.3%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-28c6f3cbbc37419ba606fc6727ae7467
출처 데이터셋
uspto-grants-1993_10
특허 번호
US05256800

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