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

HRID 1246624
ノート
印刷プレビュー

反応式

HRID 1246624 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 2M HCl and stirred for a further 30 min. The mixture was then basified by the addition of 2M NaOH until pH 10 was attained. The mixture was then washed with EtOAc (3×50 mL). The aqueous layer was re-acidified by the addition of 2M HCl to pH 1 and extracted with EtOAc (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 (CDCl3, 400 MHz) 2.21 (3H, s), 3.70 (3H, s), 6.30 (1H, d), 6.35 (1H, s), 6.96 (1H, d), 9.39 (1H, brs).

後処理

  1. customwas quenched with 2M HCl
  2. stirringstirred for a further 30 min
  3. additionThe mixture was then basified by the addition of 2M NaOH until pH 10
  4. washThe mixture was then washed with EtOAc (3×50 mL)
  5. additionThe aqueous layer was re-acidified by the addition of 2M HCl to pH 1
  6. extractionextracted with EtOAc (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-06e630104681478e9148516800170974
出典データセット
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07129234B2

反応ノート

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