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

HRID 735021노트

반응식

HRID 735021 반응식
[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

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 68816272HCID 68816272, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7cb56a56b8b74a6f8a74a5f55b8cb919
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07592373B2

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