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Sodium Hydroxide → HCID 21055336, 화합물

HRID 2215266
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HRID 2215266 반응식
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]
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참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 23642ThioguaiacolHCID 10986449(S)-(+)-3-Bromo-2-methyl-1-propanol

생성물 1

HCID 21055336HCID 21055336, 화합물수율 100%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-ffb14ca1d77e45778e3c3835d462584c
출처 데이터셋
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07109234B2

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