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Sodium Hydroxide → HCID 21055336、化合物

HRID 2215266
ノート
印刷プレビュー

反応式

HRID 2215266 の反応式
Br[CH2:2][C@@H:3]([CH3:6])[CH2:4][OH:5].[OH-].[Na+].[CH3:9][O:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[SH:17]>O>[CH3:6][C@H:3]([CH2:2][S:17][C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=1[O:10][CH3:9])[CH2:4][OH:5]
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 14798Sodium HydroxideHCID 23642ThioguaiacolHCID 10986449(S)-(+)-3-Bromo-2-methyl-1-propanol

生成物 1

HCID 21055336HCID 21055336、化合物収率 100%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

2.2 ml (0.021 mol) of 3-bromo-2-(S)-methyl-1-propanol are introduced into a round-bottomed flask kept under an inert atmosphere. 20 ml of an aqueous sodium hydroxide solution (1N) are added dropwise, followed by 2.3 ml (0.019 mol) of 2-methoxythiophenol. The mixture is brought to 90° C. for 4 hours and is then cooled to ambient temperature. 50 ml of water are then added and the mixture is extracted with dichloromethane. The combined organic phases are washed with brine, dried over sodium sulfate, filtered and concentrated under reduced pressure. The residue is purified by flash chromatography on silica gel (eluent: dichloromethane/methanol=99:1). 4 g (0.019 mol) of the title compound (XXb-1) are recovered in the form of a colorless oil.

後処理

  1. extractionthe mixture is extracted with dichloromethane
  2. washThe combined organic phases are washed with brine
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe residue is purified by flash chromatography on silica gel (eluent: dichloromethane/methanol=99:1)

出典と根拠

ORDレコード
ord-ffb14ca1d77e45778e3c3835d462584c
出典データセット
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07109234B2

反応ノート

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