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Sodium Azide → ethyl 7-(azidomethyl)-6-chloro-2-(trifluoromethyl)-2H-chromene-3-carboxylate

HRID 854892
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HRID 854892 반응식
Br[CH2:2][C:3]1[CH:12]=[C:11]2[C:6]([CH:7]=[C:8]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[CH:9]([C:13]([F:16])([F:15])[F:14])[O:10]2)=[CH:5][C:4]=1[Cl:22].[N-:23]=[N+:24]=[N-:25].[Na+]>CN(C=O)C>[N:23]([CH2:2][C:3]1[CH:12]=[C:11]2[C:6]([CH:7]=[C:8]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[CH:9]([C:13]([F:16])([F:15])[F:14])[O:10]2)=[CH:5][C:4]=1[Cl:22])=[N+:24]=[N-:25]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 33557Sodium AzideHCID 69517129ethyl 7-(bromomethyl)-6-chloro-2-(trifluoromethyl)-2H-chromene-3-carboxylate

생성물 1

HCID 86599453ethyl 7-(azidomethyl)-6-chloro-2-(trifluoromethyl)-2H-chromene-3-carboxylate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
50 °C

실험 절차

The ester from step 3 (2.2 g, 5.5 mmole) and sodium azide (1.79 g, 27.5 mmole) were dissolved in DMF (15 mL). The mixture was heated at 50° C. under nitrogen for overnight. The solid was filtered off and washed with EtOAc. The organic layer was washed with water and dried over MgSO4. After concentrated the ester was of suitable purity to use without further purification.

후처리

  1. filtrationThe solid was filtered off
  2. washwashed with EtOAc
  3. washThe organic layer was washed with water
  4. dry with materialdried over MgSO4
  5. concentrationAfter concentrated the ester
  6. customto use without further purification

출처 및 근거

ORD 기록
ord-68abea5559674609b1cc094c96b3f093
출처 데이터셋
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07259266B2

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