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Lithium azide → HCID 19781831, 화합물

HRID 257844
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HRID 257844 반응식
Br[CH2:2][C:3]1[CH:21]=[CH:20][C:6]([O:7][CH:8]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=2[Cl:19])[C:9]([O:11][CH3:12])=[O:10])=[CH:5][CH:4]=1.[N-:22]=[N+:23]=[N-:24].[Li+]>CS(C)=O>[N:22]([CH2:2][C:3]1[CH:21]=[CH:20][C:6]([O:7][CH:8]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=2[Cl:19])[C:9]([O:11][CH3:12])=[O:10])=[CH:5][CH:4]=1)=[N+:23]=[N-:24]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 88163Lithium azideHCID 19385740Methyl 2-(4-bromomethylphenoxy)-2-(2-chlorophenyl)acetate

생성물 1

HCID 19781831HCID 19781831, 화합물

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

A concentrated stirred solution of the product of Step D in anhydrous dimethylsulfoxide (DMSO) is treated at ambient temperature with lithium azide (25% excess) portionwise. The mixture is then stirred at ambient temperature under protection from moisture for about 1 hour, or until TLC indicates complete reaction. The mixture is then partitioned between ether (or ethyl acetate) and water. The organic phase is washed repeatedly with H2O, then dried over MgSO4, filtered, and concentrated. The residue may be purified by chromatography on silica gel.

후처리

  1. customreaction
  2. customThe mixture is then partitioned between ether (or ethyl acetate) and water
  3. washThe organic phase is washed repeatedly with H2O
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe residue may be purified by chromatography on silica gel

출처 및 근거

ORD 기록
ord-1b82ed8b64124b7ba5b4aa181854c014
출처 데이터셋
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05264439

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