Hydrochloric Acid → N-{2-Amino-1-[3-(trifluoromethyl)phenyl]ethyl}-2-{3-(4-chlorophenyl)-5-oxo-4-[(2S)-3,3,3-trifluoro-2-hydroxypropyl]-4,5-dihydro-1H-1,2,4-triazol-1-yl}acetamide hydrochloride

HRID 2402834

反応式

HRID 2402834 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:12]([CH2:13][C@H:14]([OH:19])[C:15]([F:18])([F:17])[F:16])[C:11](=[O:20])[N:10]([CH2:21][C:22]([NH:24][CH:25]([C:30]3[CH:35]=[CH:34][CH:33]=[C:32]([C:36]([F:39])([F:38])[F:37])[CH:31]=3)[CH2:26][N+:27]([O-])=O)=[O:23])[N:9]=2)=[CH:4][CH:3]=1.[In].Cl>C1COCC1>[ClH:1].[NH2:27][CH2:26][CH:25]([NH:24][C:22](=[O:23])[CH2:21][N:10]1[C:11](=[O:20])[N:12]([CH2:13][C@H:14]([OH:19])[C:15]([F:18])([F:16])[F:17])[C:8]([C:5]2[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=2)=[N:9]1)[C:30]1[CH:35]=[CH:34][CH:33]=[C:32]([C:36]([F:38])([F:37])[F:39])[CH:31]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 5359967IndiumHCID 469292312-{3-(4-Chlorophenyl)-5-oxo-4-[(2S)-3,3,3-trifluoro-2-hydroxypropyl]-4,5-dihydro-1H-1,2,4-triazol-1-yl}-N-{2-nitro-1-[3-(trifluoromethyl)phenyl]ethyl}acetamide

生成物 1

HCID 46929233N-{2-Amino-1-[3-(trifluoromethyl)phenyl]ethyl}-2-{3-(4-chlorophenyl)-5-oxo-4-[(2S)-3,3,3-trifluoro-2-hydroxypropyl]-4,5-dihydro-1H-1,2,4-triazol-1-yl}acetamide hydrochloride

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Of the compound from Example 1, 45 mg (77 μmol) and 40 mg (348 μmol) of indium powder were admixed in 0.5 ml of THF with 42 μl of conc. hydrochloric acid, and the mixture was stirred at RT for 2 h. Then the mixture was purified by preparative HPLC (Method 10). The product-containing fractions were admixed with 2 ml of 1N hydrochloric acid and concentrated on a rotary evaporator. Drying in an HV gave 21 mg (46% of theory) of the title compound as a diastereomer mixture.

後処理

  1. customThen the mixture was purified by preparative HPLC (Method 10)
  2. concentrationconcentrated on a rotary evaporator
  3. customDrying in an HV

出典と根拠

ORDレコード
ord-5179967580664d8a857c85baa363b240
出典データセット
uspto-grants-2014_08
特許番号
US08796324B2

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