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Tert-Butylamine → N-(tert-butyl)(dimethyl)(2-methyl-8H-indeno[2,1-b]thiophen-8-yl)silanamine

HRID 1868546
ノート
印刷プレビュー

反応式

HRID 1868546 の反応式
[C:1]([NH2:5])([CH3:4])([CH3:3])[CH3:2].[Li]CCCC.Cl[Si:12]([CH3:27])([CH3:26])[CH:13]1[C:21]2[S:22][C:23]([CH3:25])=[CH:24][C:20]=2[C:19]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]1=2>CCOCC.CCCCCC>[C:1]([NH:5][Si:12]([CH3:26])([CH3:27])[CH:13]1[C:21]2[S:22][C:23]([CH3:25])=[CH:24][C:20]=2[C:19]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]1=2)([CH3:4])([CH3:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6385Tert-ButylamineHCID 58931541chloro(dimethyl)(2-methyl-8H-indeno[2,1-b]thiophen-8-yl)silaneHCID 178418339Butyllithium

生成物 1

HCID 11985223N-(tert-butyl)(dimethyl)(2-methyl-8H-indeno[2,1-b]thiophen-8-yl)silanamine

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒2 回
HCID 8058
Hexane
溶媒

実験手順

A solution of 0.93 mL (0.0089 mol) of tert-butylamine in 30 mL of ether was treated dropwise with 5.55 mL (0.0089 mol) of 1.6M BuLi in hexane at −30° C. The reaction mixture was stirred at r.t. for 3 h and the resulting suspension was treated with a solution of 2.47 g (0.0088 mol) of chloro(dimethyl)(2-methyl-8H-indeno[2,1-b]thiophen-8-yl)silane in 10 mL of ether at −70° C. The resulting suspension was allowed to warm to r.t. and was stirred overnight. The solution was separated from LiCl and evaporated. The residue was treated with 60 mL hexane, the solution was isolated and evaporated. Yield 1.98 g (71%) of crude product as red oil.

後処理

  1. temperatureto warm to r.t.
  2. stirringwas stirred overnight
  3. customThe solution was separated from LiCl
  4. customevaporated
  5. additionThe residue was treated with 60 mL hexane
  6. customthe solution was isolated
  7. customevaporated

出典と根拠

ORDレコード
ord-299023cbf0484a6a83fcca64f5cc6865
出典データセット
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07635781B2

反応ノート

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