Imidazole → tert-Butyl-(5-tert-butyl-2-methyl-4-thiocyanato-phenoxy)-dimethyl-silane

HRID 1003857ノート

反応式

HRID 1003857 の反応式
[C:1]([C:5]1[C:6]([S:13][C:14]#[N:15])=[CH:7][C:8]([CH3:12])=[C:9]([OH:11])[CH:10]=1)([CH3:4])([CH3:3])[CH3:2].N1C=CN=C1.CN(C=O)C.[Si:26](Cl)([C:29]([CH3:32])([CH3:31])[CH3:30])([CH3:28])[CH3:27]>C(=O)(O)[O-].[Na+]>[C:29]([Si:26]([O:11][C:9]1[CH:10]=[C:5]([C:1]([CH3:4])([CH3:2])[CH3:3])[C:6]([S:13][C:14]#[N:15])=[CH:7][C:8]=1[CH3:12])([CH3:28])[CH3:27])([CH3:32])([CH3:31])[CH3:30]

参加物

6

反応物 4

HCID 795ImidazoleHCID 6228DimethylformamideHCID 28928tert-Butyldimethylsilyl chlorideHCID 105609555-tert-Butyl-2-methyl-4-thiocyanato-phenol

生成物 1

HCID 18798714tert-Butyl-(5-tert-butyl-2-methyl-4-thiocyanato-phenoxy)-dimethyl-silane

試薬・触媒・溶媒 1

HCID 516892Sodium Bicarbonate溶媒

実験手順

A solution of 2.0 g (9.0 mmol) of 5-tert-butyl-2-methyl-4-thiocyanato-phenol (prepared in Example GGG), imidazole (0.800 g, 11.8 mmol) and DMF (10 mL) was treated with t-butyldimethylsilylchloride (1.64 g, 10.9 mmol) and stirred overnight. The mixture was diluted with saturated sodium bicarbonate and the mixture extracted with hexanes. The hexane layers were combined, dried (Na2SO4), and the solvent removed in vacuo to yield the title compound. 1H NMR (CDCl3) δ 0.23 (s, 6 H), 1.01 (s, 9 H), 1.45 (s, 9 H), 2.16 (s, 3 H), 6.87 (s, 1 H), 7.49 (s, 1 H).

後処理

  1. extractionthe mixture extracted with hexanes
  2. dry with materialdried (Na2SO4)
  3. customthe solvent removed in vacuo

出典と根拠

ORDレコード
ord-ea5f2c837654414bbaa6d220b49f3caa
出典データセット
uspto-grants-2000_04
特許番号
US06046355

反応ノート

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