Trifluoroacetic acid → HCID 178522004, 화합물

HRID 1521770노트

반응식

HRID 1521770 반응식
[O:1]=[C:2]1[NH:8][CH2:7][CH2:6][CH2:5][N:4]2[C:9]3[N:15]=[C:14]([C:16]([NH:18][C:19]4[CH:24]=[CH:23][CH:22]=[C:21]([C:25]5[N:26]=[CH:27][N:28](C(C6C=CC=CC=6)(C6C=CC=CC=6)C6C=CC=CC=6)[CH:29]=5)[CH:20]=4)=[O:17])[CH:13]=[CH:12][C:10]=3[CH:11]=[C:3]12.C(O)(C(F)(F)F)=O>C(Cl)Cl>[NH:28]1[CH:29]=[C:25]([C:21]2[CH:20]=[C:19]([NH:18][C:16]([C:14]3[CH:13]=[CH:12][C:10]4[CH:11]=[C:3]5[C:2](=[O:1])[NH:8][CH2:7][CH2:6][CH2:5][N:4]5[C:9]=4[N:15]=3)=[O:17])[CH:24]=[CH:23][CH:22]=2)[N:26]=[CH:27]1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 672372246-oxo-N-[3-(1-trityl-1H-imidazol-4-yl)phenyl]-7,8,9,10-tetrahydro-6H-pyrido[3',2':4,5]pyrrolo[1,2-a][1,4]diazepine-2-carboxamide

생성물 1

HCID 178522004HCID 178522004, 화합물수율 47%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 6-oxo-N-[3-(1-trityl-1H-imidazol-4-yl)phenyl]-7,8,9,10-tetrahydro-6H-pyrido[3′,2′:4,5]pyrrolo[1,2-a][1,4]diazepine-2-carboxamide (86 mg, 0.14 mmol) in CH2Cl2 (1 mL) is added TFA (0.5 mL). The mixture is stirred at room temperature for 16 hr then is concentrated under reduced pressure. The residue is purified via preparative HPLC using a gradient elution from 10-75% acetonitrile/H2O with 0.1% TFA to afford the title compound (25 mg, 47%). LCMS: 387.86 (M+H+). (System T-med polar) Table 3 below, lists the mass spectral data and the HPLC retention times for Examples 1 to 105.

후처리

  1. concentrationthen is concentrated under reduced pressure
  2. customThe residue is purified via preparative HPLC
  3. washa gradient elution from 10-75% acetonitrile/H2O with 0.1% TFA

출처 및 근거

ORD 기록
ord-38eec52f48b748628f162095f25007be
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09073926B2

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