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

HRID 1279639
ノート
印刷プレビュー

反応式

HRID 1279639 の反応式
[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]
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 6343EthanethiolHCID 7657Dibenzyl etherHCID 8000Boron trifluoride etherate

生成物 1

HCID 218771303-Methoxy-4-(methylsulfanyl)phenol収率 28%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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)

後処理

  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)]

出典と根拠

ORDレコード
ord-7fbc993ea7484477afab05404781d4c2
出典データセット
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06448293B1

反応ノート

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