Potassium Carbonate → tert-butyl (NE)-N-[[3-(trifluoromethyl)phenyl]methylidene]carbamate

HRID 2402767

반응식

HRID 2402767 반응식
C(=O)([O-])[O-].[K+].[K+].C1(S([CH:16]([NH:27][C:28](=[O:34])[O:29][C:30]([CH3:33])([CH3:32])[CH3:31])[C:17]2[CH:22]=[CH:21][CH:20]=[C:19]([C:23]([F:26])([F:25])[F:24])[CH:18]=2)(=O)=O)C=CC=CC=1>C1COCC1>[F:24][C:23]([F:25])([F:26])[C:19]1[CH:18]=[C:17](/[CH:16]=[N:27]/[C:28](=[O:34])[O:29][C:30]([CH3:33])([CH3:31])[CH3:32])[CH:22]=[CH:21][CH:20]=1

참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 59536907tert-Butyl {(phenylsulphonyl)[3-(trifluoromethyl)phenyl]methyl}carbamate

생성물 1

HCID 46855703tert-butyl (NE)-N-[[3-(trifluoromethyl)phenyl]methylidene]carbamate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A quantity of 10.88 g (78.73 mmol) of potassium carbonate was dried hot in an HV, left to cool under argon to RT and admixed with 127 ml of THF and also with 5.45 g (13.12 mmol) of the sulphonyl compound from Example 10A. The mixture was stirred at reflux for 16 h under argon. The mixture was cooled to RT and then filtered through Celite. The latter was rinsed with THF. The entire filtrate was freed from the volatile components on a rotary evaporator and then in an HV, to give 3.63 g (100% of theory) of the title compound.

후처리

  1. waitleft
  2. temperatureat reflux for 16 h under argon
  3. temperatureThe mixture was cooled to RT
  4. filtrationfiltered through Celite
  5. washThe latter was rinsed with THF
  6. customThe entire filtrate was freed from the volatile components on a rotary evaporator

출처 및 근거

ORD 기록
ord-83a6e27bdf024bdaa0ef4e2cc4edd2ac
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08796324B2

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