Trifluoroacetic acid → HCID 178522004、化合物

HRID 1521770ノート

反応式

HRID 1521770 の反応式
[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

参加物

4

反応物 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

生成物 1

HCID 178522004HCID 178522004、化合物収率 47%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-38eec52f48b748628f162095f25007be
出典データセット
uspto-grants-2015_07
特許番号
US09073926B2

反応ノート

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