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Methanol → (2'-Fluoro-4-(hydroxymethyl)-5'-(methyloxy)-1,1'-biphenyl-2-yl)(1-methylcyclopropyl)methanol

HRID 1662534
ノート
印刷プレビュー

反応式

HRID 1662534 の反応式
CC([Si](C)(C)[O:6][CH2:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]2[CH:19]=[C:18]([O:20][CH3:21])[CH:17]=[CH:16][C:15]=2[F:22])=[C:10]([CH:23]([C:25]2([CH3:28])[CH2:27][CH2:26]2)[OH:24])[CH:9]=1)(C)C.CO.CC1C=CC(S([O-])(=O)=O)=CC=1.C1C=C[NH+]=CC=1>CCOC(C)=O>[F:22][C:15]1[CH:16]=[CH:17][C:18]([O:20][CH3:21])=[CH:19][C:14]=1[C:11]1[CH:12]=[CH:13][C:8]([CH2:7][OH:6])=[CH:9][C:10]=1[CH:23]([C:25]1([CH3:28])[CH2:27][CH2:26]1)[OH:24]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 887MethanolHCID 466102Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1)HCID 57706611(4-((((1,1-Dimethylethyl)(dimethyl)silyl)oxy)methyl)-2'-fluoro-5'-(methyloxy)-1,1'-biphenyl-2-yl)(1-methylcyclopropyl)methanol

生成物 1

HCID 57706703(2'-Fluoro-4-(hydroxymethyl)-5'-(methyloxy)-1,1'-biphenyl-2-yl)(1-methylcyclopropyl)methanol収率 88%

試薬・触媒・溶媒 1

HCID 8857
Ethyl Acetate
溶媒

実験手順

A 200 mL round bottom flask was charged with 83.18E (0.80 g, 1.9 mmol), MeOH (10 mL), and PPTS (0.047 g, 0.19 mmol). The solution was stirred overnight at room temperature and diluted with EtOAc. The organic phase was washed with water and brine, dried (MgSO4), and concentrated. The crude product was purified by silica gel flash chromatography (20-55% EtOAc/hexane) to afford 83.18F (0.52 g, 88%) as a colorless oil.

後処理

  1. washThe organic phase was washed with water and brine
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated
  4. customThe crude product was purified by silica gel flash chromatography (20-55% EtOAc/hexane)

出典と根拠

ORDレコード
ord-71bef6b37622477a943012288f7d3bfe
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08030354B2

反応ノート

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