Trifluoroacetic acid → HCID 57265194、化合物

HRID 1941428ノート

反応式

HRID 1941428 の反応式
[C:1]1([S:7]([CH2:10][NH:11][C:12]2[C:20]3[C:15](=[CH:16][C:17]([Cl:29])=[C:18](C(OC(C)(C)C)=O)[C:19]=3[Cl:21])[NH:14][C:13]=2[C:30]([O:32][CH2:33][CH3:34])=[O:31])(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.FC(F)(F)C(O)=O>C(Cl)Cl>[C:1]1([S:7]([CH2:10][NH:11][C:12]2[C:20]3[C:15](=[CH:16][C:17]([Cl:29])=[CH:18][C:19]=3[Cl:21])[NH:14][C:13]=2[C:30]([O:32][CH2:33][CH3:34])=[O:31])(=[O:8])=[O:9])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 67705862HCID 67705862、化合物

生成物 1

HCID 57265194HCID 57265194、化合物収率 22%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Dissolve 3-[(phenylsulfonyl)methylamino]-2-carbethoxy-4,6-dichloro-tert-butyloxycarbonyl-indole (400 mg, 0.758 mmol) in methylene chloride (15 mL). Add, by dropwise addition, trifluoroacetic acid (15 mL) and stir at room temperature for 3 hours. Evaporate the solvent in vacuo and treat the resulting residue with saturated sodium hydrogen carbonate. Extact into methylene chloride and dry (MgSO4). Recrystallize (ethyl acetate/hexane) to give the title compound (70 mg, 22%); mp 244°-45° C.

後処理

  1. customEvaporate the solvent in vacuo
  2. additiontreat the resulting residue with saturated sodium hydrogen carbonate
  3. dry with materialExtact into methylene chloride and dry (MgSO4)
  4. customRecrystallize (ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-1b86c02b55324c8f90d40a2b93a71da5
出典データセット
uspto-grants-1997_12
特許番号
US05703107

反応ノート

読み込み中…