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

HRID 853119
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HRID 853119 반응식
[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]
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참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 3283Diethyl Ether용매2회
HCID 8058
Hexane
용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1e03c3de0a544caeae4f5be5a6f38d62
출처 데이터셋
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07253292B2

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