Trifluoroacetic acid → HCID 15231616、化合物

HRID 258042ノート

反応式

HRID 258042 の反応式
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]

参加物

4

反応物 2

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

生成物 1

HCID 15231616HCID 15231616、化合物収率 98.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 3-tert-butyloxycarbonylamino-4-(2-methylphenyl)-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.

後処理

  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

出典と根拠

ORDレコード
ord-d93613a7591841e4aa6868f13bb9c091
出典データセット
uspto-grants-1993_11
特許番号
US05264454

反応ノート

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