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

HRID 2098269노트

반응식

HRID 2098269 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) is added at 0° C. to a stirred solution of (tert-butoxy)-N-{4-[(fluoren-9-ylmethoxy)carbonylamino]phenyl}carboxamide (20.60 g, 47.85 mmol, 1.0 eq) in CH2Cl2 (900 mL). The resulting solution is allowed to warm to room temperature. After stirring overnight at room temperature, the reaction mixture is concentrated to dryness and the residue is triturated in water. Then the mixture is filtered to afford 15.80 g of the expected crude product as a white powder.

후처리

  1. concentrationthe reaction mixture is concentrated to dryness
  2. customthe residue is triturated in water
  3. filtrationThen the mixture is filtered

출처 및 근거

ORD 기록
ord-68db198bd6bf422aa561091dc14b6ab5
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08450477B2

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