Potassium Carbonate → tert-butyl (NE)-N-[(2-chlorophenyl)methylidene]carbamate

HRID 2402794노트

반응식

HRID 2402794 반응식
C(=O)([O-])[O-].[K+].[K+].[Cl:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[CH:14]([NH:24][C:25](=[O:31])[O:26][C:27]([CH3:30])([CH3:29])[CH3:28])S(C1C=CC=CC=1)(=O)=O>C1COCC1>[Cl:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1/[CH:14]=[N:24]/[C:25](=[O:31])[O:26][C:27]([CH3:29])([CH3:28])[CH3:30]

참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 59536806tert-Butyl [(2-chlorophenyl)(phenylsulphonyl)methyl]carbamate

생성물 1

HCID 12195069tert-butyl (NE)-N-[(2-chlorophenyl)methylidene]carbamate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A quantity of 12.53 g (90.7 mmol) of potassium carbonate was heated through in an HV and then cooled under an argon atmosphere. Quantities of 140 ml of anhydrous THF and 5.77 g (15.1 mmol) of the compound from Example 110A were added and the mixture was stirred under an argon atmosphere at reflux temperature for 16 h. After cooling to RT, the reaction mixture was filtered over celite. The solid was washed with a little THF. The entire filtrate was freed from the solvent on a rotary evaporator. The oily residue was dried in an HV. This gave 3.55 g (98% of theory) of the title compound.

후처리

  1. temperaturecooled under an argon atmosphere
  2. temperatureat reflux temperature for 16 h
  3. filtrationthe reaction mixture was filtered over celite
  4. washThe solid was washed with a little THF
  5. customThe entire filtrate was freed from the solvent on a rotary evaporator
  6. customThe oily residue was dried in an HV

출처 및 근거

ORD 기록
ord-4052e54b6f294235af11cd7e02ca4bb7
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08796324B2

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