Potassium Phosphate, Dibasic → 2-tert-Butyl-4-(tert-butyl-dimethyl-silanyloxy)-5-methyl-benzenethiol

HRID 356502ノート

反応式

HRID 356502 の反応式
[C:1]([Si:5]([O:8][C:9]1[CH:14]=[C:13]([C:15]([CH3:18])([CH3:17])[CH3:16])[C:12]([S:19]C#N)=[CH:11][C:10]=1[CH3:22])([CH3:7])[CH3:6])([CH3:4])([CH3:3])[CH3:2].SC[C@H]([C@@H](CS)O)O.OP([O-])([O-])=O.[K+].[K+]>CCO>[C:15]([C:13]1[CH:14]=[C:9]([O:8][Si:5]([C:1]([CH3:4])([CH3:3])[CH3:2])([CH3:6])[CH3:7])[C:10]([CH3:22])=[CH:11][C:12]=1[SH:19])([CH3:18])([CH3:17])[CH3:16]

参加物

5

反応物 3

HCID 24450Potassium Phosphate, DibasicHCID 446094D-1,4-DithiothreitolHCID 18798714tert-Butyl-(5-tert-butyl-2-methyl-4-thiocyanato-phenoxy)-dimethyl-silane

生成物 1

HCID 187986992-tert-Butyl-4-(tert-butyl-dimethyl-silanyloxy)-5-methyl-benzenethiol

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 3.02 g (9.00 mmol) of tert-butyl-(5-tert-butyl-2-methyl-4-thiocyanato-phenoxy)-dimethyl-silane (prepared in Example HHH), 2.3 g (12 mmol) of dithiothreitol, EtOH (20 mL), and 0.02M potassium dibasic phosphate buffer (10 mL) was heated to 50° C. overnight. The mixture was cooled to room temperature, diluted with hexanes and washed with H2O. The organic layer was then dried (Na2SO4) and the solvent removed in vacuo to yield the title compound. 1H NMR (CDCl3) δ 0.20 (s, 6 H), 1.00 (s, 9 H), 1.44 (s, 9 H), 2.10 (s, 3 H), 3.42 (s, 1 H), 6.80 (s, 1 H), 7.04 (s, 1 H).

後処理

  1. customwas heated to 50° C. overnight
  2. washwashed with H2O
  3. dry with materialThe organic layer was then dried (Na2SO4)
  4. customthe solvent removed in vacuo

出典と根拠

ORDレコード
ord-3af43cbe6ef14515b46d020d771b9a53
出典データセット
uspto-grants-1998_11
特許番号
US05834506

反応ノート

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