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Ethanethiol → 3-Methoxy-4-(methylsulfanyl)phenol

HRID 1279639
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HRID 1279639 반응식
[CH2:1]([O:8]CC1C=CC=CC=1)[C:2]1C=CC=[CH:4][CH:3]=1.[CH2:16]([SH:18])C.B(F)(F)F.C[CH2:24][O:25][CH2:26][CH3:27]>C(Cl)Cl>[CH3:24][O:25][C:26]1[CH:27]=[C:1]([OH:8])[CH:2]=[CH:3][C:4]=1[S:18][CH3:16]
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참가 물질

5

반응물 3

HCID 6343EthanethiolHCID 7657Dibenzyl etherHCID 8000Boron trifluoride etherate

생성물 1

HCID 218771303-Methoxy-4-(methylsulfanyl)phenol수율 28%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

The benzylether from stage (iii) (9.27 g, 39.5 mmol) was dissolved in DCM (5 mL), ethanethiol (5 mL) and BF3.OEt2 (5 mL, 39.5 mol) were then added at room temperature under a nitrogen atmosphere. The mixture was stirred overnight before the reaction was quenched with hydrochloric acid (2 M) and stirred for a further 30 mins. The mixture was then basified by the addition of sodium hydroxide (2 M) until pH 10 was attained. The mixture was then washed with ethyl acetate (3×50 mL). The aqueous layer was reacidified by the addition of hydrochloric acid (2 M) to pH 1 and extracted with ethyl acetate (4×50 mL). The extracts were combined, dried (MgSO4) and evaporated to an oil. Purification by flash chromatography [SiO2; EtOAc/ pentane (1:9→1:4)] afforded the desired phenol compound as a colourless solid (1.73 g, 28%); δH(CDCI3, 400 MHz) 2.21 (3 H, s), 3.70 (3 H, s), 6.30 (1 H, d), 6.35 (1 H, s), 6.96 (1 H, d), 9.39 (1 H, brs)

후처리

  1. customwas quenched with hydrochloric acid (2 M)
  2. stirringstirred for a further 30 mins
  3. additionThe mixture was then basified by the addition of sodium hydroxide (2 M) until pH 10
  4. washThe mixture was then washed with ethyl acetate (3×50 mL)
  5. additionThe aqueous layer was reacidified by the addition of hydrochloric acid (2 M) to pH 1
  6. extractionextracted with ethyl acetate (4×50 mL)
  7. dry with materialdried (MgSO4)
  8. customevaporated to an oil
  9. customPurification by flash chromatography [SiO2; EtOAc/ pentane (1:9→1:4)]

출처 및 근거

ORD 기록
ord-7fbc993ea7484477afab05404781d4c2
출처 데이터셋
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06448293B1

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