3-(Methylthio)-1-propanol → (3-(3-Bromo-2-methylphenoxy)propyl)(methyl)sulfane

HRID 237499

반응식

HRID 237499 반응식
[Br:1][C:2]1[C:3]([CH3:9])=[C:4]([OH:8])[CH:5]=[CH:6][CH:7]=1.[CH3:10][S:11][CH2:12][CH2:13][CH2:14]O.C(P(CCCC)CCCC)CCC.N(C(N1CCCCC1)=O)=NC(N1CCCCC1)=O>O1CCCC1.O>[Br:1][C:2]1[C:3]([CH3:9])=[C:4]([CH:5]=[CH:6][CH:7]=1)[O:8][CH2:14][CH2:13][CH2:12][S:11][CH3:10]

참가 물질

7

반응물 4

HCID 104483-(Methylthio)-1-propanolHCID 13831TributylphosphineHCID 730421,1'-(Azodicarbonyl)dipiperidineHCID 111714303-Bromo-2-methylphenol

생성물 1

HCID 86697160(3-(3-Bromo-2-methylphenoxy)propyl)(methyl)sulfane

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

3-Bromo-2-methylphenol (0.10 g), 3-(methylthio)propanol (0.055 mL), tri-n-butyl phosphine (0.12 g) and 1,1′-(azodicarbonyl)dipiperidine (0.15 g) are stirred in tetrahydrofurane for 16 hours. Water is added and the mixture extracted with diethyl ether. The organic layer is washed with brine, dried (Na2SO4) and volatiles removed under reduced pressure. The product (80 mg) is obtained after column chromatography (silica gel, n-hexane/ethyl acetate gradient 100:0 to 50:50).

후처리

  1. extractionthe mixture extracted with diethyl ether
  2. washThe organic layer is washed with brine
  3. dry with materialdried (Na2SO4)
  4. customvolatiles removed under reduced pressure

출처 및 근거

ORD 기록
ord-ef70e29ed21546b2a8527d437f2c62ee
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08642585B2

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