Trifluoroacetic acid → HCID 15231616, 화합물

HRID 36935노트

반응식

HRID 36935 반응식
C(OC([NH:8][C:9]1[C:10](=[O:29])[O:11][C:12]2[CH:25]=[C:24]3[CH2:26][CH2:27][CH2:28][C:23]3=[CH:22][C:13]=2[C:14]=1[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[CH3:21])=O)(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[NH2:8][C:9]1[C:10](=[O:29])[O:11][C:12]2[CH:25]=[C:24]3[CH2:26][CH2:27][CH2:28][C:23]3=[CH:22][C:13]=2[C:14]=1[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[CH3:21]

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 197821663-tert-butyloxycarbonylamino-4-(2-methylphenyl)-7,8-dihydro-6H-cyclopenta[g][1]benzopyran-2-one

생성물 1

HCID 15231616HCID 15231616, 화합물수율 98.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 3-tert-butyloxycarbonylamino-4-(2methylphenyl) -7,8-dihydro-6H-cyclopenta [g] [1 ]benzopyran-2-one (2.05 g) in dichloromethane (20 ml) was added trifluoroacetic acid (10 ml) dropwise with ice-cooling. The mixture was stirred under ice-cooling for 1 hour, after which the solvent was distilled off. The residue was diluted with water, neutralized with saturated aqueous solution of NaHCO3 and extracted with chloroform. The extract was washed with water and dried (MgSO4) and the solvent was distilled off to give crystals of 3-amino-4-(2-methylphenyl)-7,8-dihydro-6H-cyclopenta[g] [1]-benzopyran-2-one (1.5 g, 98.4%). Recrystallization from ethanol-dichloromethane gave colorless prisms, m.p. 275°-276° C.

후처리

  1. temperaturecooling
  2. temperaturecooling for 1 hour
  3. distillationafter which the solvent was distilled off
  4. additionThe residue was diluted with water
  5. extractionextracted with chloroform
  6. washThe extract was washed with water
  7. dry with materialdried (MgSO4)
  8. distillationthe solvent was distilled off

출처 및 근거

ORD 기록
ord-ef64be96741b445a80d575ce071b802a
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05418239

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