Trifluoroacetic acid → (9H-Fluoren-9-yl)methyl (4-aminophenyl)carbamate

HRID 527385노트

반응식

HRID 527385 반응식
C(O)(C(F)(F)F)=O.C(OC([NH:15][C:16]1[CH:21]=[CH:20][C:19]([NH:22][C:23]([O:25][CH2:26][CH:27]2[C:39]3[CH:38]=[CH:37][CH:36]=[CH:35][C:34]=3[C:33]3[C:28]2=[CH:29][CH:30]=[CH:31][CH:32]=3)=[O:24])=[CH:18][CH:17]=1)=O)(C)(C)C>C(Cl)Cl>[NH2:15][C:16]1[CH:17]=[CH:18][C:19]([NH:22][C:23]([O:25][CH2:26][CH:27]2[C:39]3[CH:38]=[CH:37][CH:36]=[CH:35][C:34]=3[C:33]3[C:28]2=[CH:29][CH:30]=[CH:31][CH:32]=3)=[O:24])=[CH:20][CH:21]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 131730600HCID 131730600, 화합물

생성물 1

HCID 11450338(9H-Fluoren-9-yl)methyl (4-aminophenyl)carbamate수율 99.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

TFA (55.30 mL, 717.76 mmol, 15.0 eq) was added at 0° C. to a stirred solution of (tert-butoxy)-N-{4-[(fluoren-9-yl-methoxy)carbonylamino]phenyl}carboxamide (20.60 g, 47.85 mmol, 1.0 eq) in CH2Cl2 (900 mL). The resulting solution was allowed to come at room temperature. After stirring overnight at room temperature, the reaction mixture was concentrated to dryness and the residue was triturated in water. Then the mixture was filtered to afford 15.80 g of the expected crude product as a white powder.

후처리

  1. customto come at room temperature
  2. concentrationthe reaction mixture was concentrated to dryness
  3. customthe residue was triturated in water
  4. filtrationThen the mixture was filtered

출처 및 근거

ORD 기록
ord-99f524d309bc41718bcb41e42f20fd6b
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09346799B2

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