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Sodium Azide → HCID 57976173, 화합물

HRID 1865322
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HRID 1865322 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:12](=[O:13])[C:11]([CH2:15]OS(C)(=O)=O)([CH3:14])[NH:10][C:9]2=[O:21])=[CH:4][C:3]=1[C:22]([F:25])([F:24])[F:23].[N-:26]=[N+:27]=[N-:28].[Na+]>CN(C=O)C>[N:26]([CH2:15][C:11]1([CH3:14])[NH:10][C:9](=[O:21])[N:8]([C:5]2[CH:6]=[CH:7][C:2]([Cl:1])=[C:3]([C:22]([F:25])([F:23])[F:24])[CH:4]=2)[C:12]1=[O:13])=[N+:27]=[N-:28]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 33557Sodium AzideHCID 57976191HCID 57976191, 화합물

생성물 1

HCID 57976173HCID 57976173, 화합물수율 65.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Methanesulfonic acid 1-(4-chloro-3-trifluoromethyl-phenyl)-4-methyl-2,5-dioxo-imidazolidin-4-ylmethyl ester (1.0 g, 2.5 mmoL) from Example 11, NaN3 (1.6 g, 25 mmoL) and KI (40 mg, 0.25 mmoL) in DMF (8 mL) was heated at 100° C. for 10 hrs. The crude product was partitioned between ether and water. The organic layer was washed with water, brine, dried over anhydrous Na2SO4, filtered and concentrated, then purified by silica gel column chromatography using heptane and ethyl acetate as eluent to afford the title compound as a colorless oil (566 mg, yield 65%).

후처리

  1. customThe crude product was partitioned between ether and water
  2. washThe organic layer was washed with water, brine
  3. dry with materialdried over anhydrous Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. custompurified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-2c52b16c8d8a4174bef75da22f1e462e
출처 데이터셋
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07626036B2

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