Trifluoroacetic acid → 3-[4-(1-aminocyclopropyl)phenyl]propynoic acid-(4'-chlorobiphenyl-4-yl)amide Trifluoroacetate

HRID 735021ノート

反応式

HRID 735021 の反応式
[F:1][C:2]([F:7])([F:6])[C:3]([OH:5])=[O:4].[Cl:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH:20]=[CH:19][C:18]([NH:21][C:22](=[O:42])[C:23]#[C:24][C:25]3[CH:30]=[CH:29][C:28]([C:31]4([NH:34]C(OC(C)(C)C)=O)[CH2:33][CH2:32]4)=[CH:27][CH:26]=3)=[CH:17][CH:16]=2)=[CH:11][CH:10]=1>ClCCl>[F:1][C:2]([F:7])([F:6])[C:3]([OH:5])=[O:4].[Cl:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH:16]=[CH:17][C:18]([NH:21][C:22](=[O:42])[C:23]#[C:24][C:25]3[CH:30]=[CH:29][C:28]([C:31]4([NH2:34])[CH2:32][CH2:33]4)=[CH:27][CH:26]=3)=[CH:19][CH:20]=2)=[CH:11][CH:10]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 68816272HCID 68816272、化合物

生成物 1

HCID 688198803-[4-(1-aminocyclopropyl)phenyl]propynoic acid-(4'-chlorobiphenyl-4-yl)amide Trifluoroacetate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

1 mL (12.92 mmol) of trifluoroacetic acid is added to a solution of 0.24 g (0.49 mmol) of 3-[4-(1-tert-butoxycarbonylaminocyclopropyl)phenyl]propynoic acid-(4′-chlorobiphenyl-4-yl)amide in 20 mL dichloromethane and stirred for 24 hours. Then the solvent is eliminated by rotary evaporation and the residue is combined with toluene and again subjected to rotary evaporation. This residue is then triturated with dichloromethane, suction filtered and dried in the air. Yield: 0.22 g (89% of theory); C24H19ClN2O*C2HF3O2 (M=500.90); calc.: molecular ion peak (M+H)+: 387 (Cl); found: molecular ion peak (M+H)+: 387 (Cl); melting point: 160° C.-164° C.

後処理

  1. customThen the solvent is eliminated by rotary evaporation
  2. customagain subjected to rotary evaporation
  3. customThis residue is then triturated with dichloromethane, suction
  4. filtrationfiltered
  5. customdried in the air

出典と根拠

ORDレコード
ord-7cb56a56b8b74a6f8a74a5f55b8cb919
出典データセット
uspto-grants-2009_09
特許番号
US07592373B2

反応ノート

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