Trifluoroacetic acid → (RS)-7-Amino-5H,7H-dibenzo[b,d]azepin-6-one

HRID 1372941ノート

反応式

HRID 1372941 の反応式
[NH2:1][CH:2]1[C:8](=[O:9])[N:7](CC2C=CC(OC)=CC=2)[C:6]2[CH:19]=[CH:20][CH:21]=[CH:22][C:5]=2[C:4]2[CH:23]=[CH:24][CH:25]=[CH:26][C:3]1=2.FC(F)(F)C(O)=O.FC(F)(F)S(O)(=O)=O.C([O-])(O)=O.[Na+]>ClCCl>[NH2:1][CH:2]1[C:8](=[O:9])[NH:7][C:6]2[CH:19]=[CH:20][CH:21]=[CH:22][C:5]=2[C:4]2[CH:23]=[CH:24][CH:25]=[CH:26][C:3]1=2

参加物

6

反応物 4

HCID 6422Trifluoroacetic acidHCID 62406Trifluoromethanesulfonic acidHCID 516892Sodium BicarbonateHCID 210725617-Amino-5-(4-methoxybenzyl)-5,7-dihydro-6H-dibenzo[b,d]azepin-6-one

生成物 1

HCID 23555091(RS)-7-Amino-5H,7H-dibenzo[b,d]azepin-6-one

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 0.1 g (0.29 mmol) (RS)-7-amino-5-(4-methoxy-benzyl)-5H,7H-dibenzo[b,d]azepin-6-one in 8 ml of dichloromethane at 0° C. temperature 0.67 ml (8.7 mmol) of trifluoroacetic acid and 0.25 ml of trifluoromethansulfonic acid (2.9 mmol) were added and the mixture was stirred for 4 hours at room temperature. After concentration of the mixture at 40° C. in vacuo an aqueous NaHCO3 solution was added and the mixture extracted two times with ethyl acetate. The combined organic layers were dried (MgSO4). After evaporation of the solvent a light yellow oil was obtained, that was used directly in the next step.

後処理

  1. extractionthe mixture extracted two times with ethyl acetate
  2. dry with materialThe combined organic layers were dried (MgSO4)
  3. customAfter evaporation of the solvent a light yellow oil
  4. customwas obtained

出典と根拠

ORDレコード
ord-904d55d679ab4a42a07d64ff57a9ce26
出典データセット
uspto-grants-2007_01
特許番号
US07160875B2

反応ノート

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