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Isopropyl chloroformate → Isopropyl 3,5-difluoro-phenylcarbamate

HRID 1179478
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HRID 1179478 반응식
C[Si]([N-][Si](C)(C)C)(C)C.[Li+].[F:11][C:12]1[CH:13]=[C:14]([CH:16]=[C:17]([F:19])[CH:18]=1)[NH2:15].Cl[C:21]([O:23][CH:24]([CH3:26])[CH3:25])=[O:22]>C1COCC1.CCOCC>[F:11][C:12]1[CH:13]=[C:14]([NH:15][C:21](=[O:22])[O:23][CH:24]([CH3:26])[CH3:25])[CH:16]=[C:17]([F:19])[CH:18]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 7917Isopropyl chloroformateHCID 965953,5-DifluoroanilineHCID 2733832Lithium hexamethyldisilazane

생성물 1

HCID 58978077Isopropyl 3,5-difluoro-phenylcarbamate

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매

실험 절차

Lithium bis(trimethylsilyl) amide (1.0 M solution in tetrahydrofuran, 542 mL, 0.542 mol) was added to a solution of 3,5-difluoroaniline (35 g, 0.271 mol) in THF (60 mL) at 0° C. Isopropyl chloroformate (1M solution in toluene, 406 mL, 0.406 mol) was then added dropwise at 0° C. and the mixture allowed to warm to room temperature over 2 h. The reaction mixture was diluted with ether and washed with 1N hydrochloric acid, water, saturated aqueous sodium bicarbonate, brine and dried (MgSO4). Solvent was removed under vacuum and the residue was triturated in hexanes to obtain the title compound.

후처리

  1. washwashed with 1N hydrochloric acid, water, saturated aqueous sodium bicarbonate, brine
  2. dry with materialdried (MgSO4)
  3. customSolvent was removed under vacuum
  4. customthe residue was triturated in hexanes

출처 및 근거

ORD 기록
ord-e00ebf9ef67c46d2949943269d0d0ab3
출처 데이터셋
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07279494B2

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