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

HRID 356502노트

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HRID 356502 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-3af43cbe6ef14515b46d020d771b9a53
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05834506

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