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

HRID 527385ノート

反応式

HRID 527385 の反応式
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

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 131730600HCID 131730600、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-99f524d309bc41718bcb41e42f20fd6b
出典データセット
uspto-grants-2016_05
特許番号
US09346799B2

反応ノート

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