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Methanol → 3-Bromo-2-methoxybenzenemethanol

HRID 1042351
ノート
印刷プレビュー

反応式

HRID 1042351 の反応式
[Li+].[BH4-].C[O:4][C:5](=O)[C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([Br:12])[C:7]=1[O:13][CH3:14].CO>CCOCC>[Br:12][C:8]1[C:7]([O:13][CH3:14])=[C:6]([CH2:5][OH:4])[CH:11]=[CH:10][CH:9]=1
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 4148881Lithium borohydrideHCID 46311082Methyl 3-bromo-2-methoxybenzoate

生成物 1

HCID 177503163-Bromo-2-methoxybenzenemethanol

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

LiBH4 (5.00 g, 0.23 mmol) was added to a solution of 3-bromo-2-methoxy-benzoic acid methyl ester (10.50 g, 42.80 mmol) in Et2O at 0° C. The reaction mixture was stirred for 5 minutes, MeOH (8.70 mL, 0.22 mmol) was added in a dropwise fashion. The reaction mixture was then stirred for 30 minutes, and was quenched into 1N NaOH. The resulting solution was extracted with Et2O (3×200 mL) and the combined organic phases were washed with brine (1×150 mL), dried over MgSO4 and concentrated to afford the title compound. Spectroscopic data: 1H NMR (300 MHz, CDCl3.) δ 1.68 (t, J=5.86 Hz, 1H), 3.90 (s, 3H), 4.61 (d, J=5.86 Hz, 2H), 6.89 (d, J=8.50 Hz, 1H), 7.25-7.30 (m, J=2.00 Hz, 1H), 7.57 (d, J=2.05 Hz, 1H).

後処理

  1. stirringThe reaction mixture was then stirred for 30 minutes
  2. customwas quenched into 1N NaOH
  3. extractionThe resulting solution was extracted with Et2O (3×200 mL)
  4. washthe combined organic phases were washed with brine (1×150 mL)
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-bf8ed33c063f48eb988d306d85c06d7e
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08557853B2

反応ノート

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