Hydrochloric Acid → HCID 86652654、化合物

HRID 43026

反応式

HRID 43026 の反応式
[F:1][C:2]([F:28])([F:27])[C:3]([NH:5][CH:6]1[C:14]2[C:9](=[CH:10][C:11]([CH2:15][N:16]3[CH:20]=[C:19]([CH2:21][OH:22])[C:18]([C:23]([F:26])([F:25])[F:24])=[N:17]3)=[CH:12][CH:13]=2)[CH2:8][CH2:7]1)=O.B#B.Cl>C1COCC1>[F:28][C:2]([F:1])([F:27])[CH2:3][NH:5][CH:6]1[C:14]2[C:9](=[CH:10][C:11]([CH2:15][N:16]3[CH:20]=[C:19]([CH2:21][OH:22])[C:18]([C:23]([F:24])([F:25])[F:26])=[N:17]3)=[CH:12][CH:13]=2)[CH2:8][CH2:7]1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 6328200DiboronHCID 445557322,2,2-Trifluoro-N-(5-((4-(hydroxymethyl)-3-(trifluoromethyl)-1H-pyrazol-1-yl)methyl)-2,3-dihydro-1H-inden-1-yl)acetamide

生成物 1

HCID 86652654HCID 86652654、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 2,2,2-trifluoro-N-(5-((4-(hydroxymethyl)-3-(trifluoromethyl)-1H-pyrazol-1-yl)methyl)-2,3-dihydro-1H-inden-1-yl)acetamide (0.172 mmol, 70 mg) in THF (2 mL) was added diborane (1.719 mmol, 1.719 mL) and the whole heated to reflux for 6 h. The reaction mixture was allowed to cool to room temperature before being treated with 2N HCl (3 mL) and left to stand overnight. After this time the crude mixture was applied to an SCX column & eluted with 2N NH3/MeOH. After evaporation, the residue was further purified by prep LCMS to give a clear film (11 mg, 0.028 mmol, 16.3%). MS (ESI): m/z [M+H]+ 394.1.

後処理

  1. temperaturethe whole heated
  2. temperatureto reflux for 6 h
  3. waitleft
  4. washeluted with 2N NH3/MeOH
  5. customAfter evaporation
  6. customthe residue was further purified by prep LCMS
  7. customto give a clear film (11 mg, 0.028 mmol, 16.3%)

出典と根拠

ORDレコード
ord-f7027af75a864385b6ed2b3a6210bce6
出典データセット
uspto-grants-2013_09
特許番号
US08536214B2

関連ノート

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