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Ammonium Hydroxide → 2,2,2-trifluoro-1-{4-[4-(1H-indazol-3-yl)-1H-1,2,3-triazol-1-yl]phenyl}ethanol

HRID 1520087
ノート
印刷プレビュー

反応式

HRID 1520087 の反応式
Br[C:2]1[CH:7]=[CH:6][C:5]([CH:8]([OH:13])[C:9]([F:12])([F:11])[F:10])=[CH:4][CH:3]=1.[C:14]([C:16]1[C:24]2[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=2)[NH:18][N:17]=1)#[CH:15].[N-:25]=[N+:26]=[N-:27].[Na+].CN[C@@H]1CCCC[C@H]1NC.[NH4+].[OH-]>CS(C)=O.O.[Cu](I)I>[F:10][C:9]([F:12])([F:11])[CH:8]([C:5]1[CH:6]=[CH:7][C:2]([N:25]2[CH:15]=[C:14]([C:16]3[C:24]4[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=4)[NH:18][N:17]=3)[N:27]=[N:26]2)=[CH:3][CH:4]=1)[OH:13]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 14923Ammonium HydroxideHCID 33557Sodium AzideHCID 2733821trans-N,N'-dimethyl-1,2-cyclohexanediamineHCID 112190241-(4-Bromophenyl)-2,2,2-trifluoroethanolHCID 178437996HCID 178437996、化合物

生成物 1

HCID 574051722,2,2-trifluoro-1-{4-[4-(1H-indazol-3-yl)-1H-1,2,3-triazol-1-yl]phenyl}ethanol
収率 26.3%

試薬・触媒・溶媒 3

HCID 83717Copper iodide触媒HCID 679Dimethyl Sulfoxide溶媒HCID 962Water溶媒

反応条件

温度
70 °C

実験手順

A mixture of 1-(4-bromophenyl)-2,2,2-trifluoroethan-1-ol (296 mg; 1.16 mmol; 1.1 eq.), 3-Ethynyl-1H-indazole (150 mg; 1.06 mmol; 1.0 eq.), sodium azide (75 mg; 1.16 mmol; 1.1 eq.), D-(−)-isoascorbic acid sodium salt (21 mg; 0.11 mmol; 0.1 eq.), copper iodide (20 mg; 0.11 mmol; 0.1 eq.) and trans-1,2-bis(methylamino)cyclohexane (22 mg; 0.16 mmol; 0.15 eq.) in DMSO (2.6 mL) and WATER (0.5 mL) was heated in a sealed tube at 70° C. for 48 h. The reaction mixture was poured into a solution of saturated NH4OH and extracted with DCM (twice). Combined organic phases were washed with brine, dried over magnesium sulfate, filtered and concentrated. Purification by preparative HPLC gave the title compound as a beige solid (100 mg, 26%). 1H NMR (DMSO) δ 13.38 (brs, 1H), 9.33 (s, 1H), 8.36 (dt, J=8.0 Hz, 1.0 Hz, 1H), 8.12 (d, J=8.7 Hz, 2H), 7.75 (d, J=8.7 Hz, 2H), 7.61 (dt, J=8.4 Hz, 1.0 Hz, 1H), 7.47-7.42 (m, 1H), 7.29-7.23 (m, 1H), 7.05 (bs, 1H), 5.34 (q, J=7.2 Hz, 1H). HPLC (max plot) 100.0%; Rt %3.83 min. UPLC/MS: (MS+) 360.4, (MS−) 358.4.

後処理

  1. extractionextracted with DCM (twice)
  2. washCombined organic phases were washed with brine
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customPurification by preparative HPLC

出典と根拠

ORDレコード
ord-afdf69e5f1a44011bc6b65118056f903
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09073892B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート