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Water → HCID 21107845, 화합물

HRID 2116804
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HRID 2116804 반응식
[C:1]([CH2:3][C:4](Cl)=[O:5])#[N:2].[CH3:7][Si:8]([CH2:19][CH2:20][CH2:21][NH2:22])([O:14][Si:15]([CH3:18])([CH3:17])[CH3:16])[O:9][Si:10]([CH3:13])([CH3:12])[CH3:11].C(N(CC)CC)C.O>ClCCl>[C:1]([CH2:3][C:4]([NH:22][CH2:21][CH2:20][CH2:19][Si:8]([CH3:7])([O:14][Si:15]([CH3:18])([CH3:17])[CH3:16])[O:9][Si:10]([CH3:13])([CH3:12])[CH3:11])=[O:5])#[N:2]
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참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 109128993-(3-Aminopropyl)heptamethyltrisiloxaneHCID 110515942-Cyanoacetyl chloride

생성물 1

HCID 21107845HCID 21107845, 화합물수율 70.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Cyanoacetyl chloride (5.2 g, 0.05 mol) is added dropwise over 20 minutes to a mixture of 3-[1,3,3,3-tetramethyl-1-[(trimethylsilyl)oxy]disiloxanyl]propylamine (13.93 g, 0.05 mol) and of triethylamine (5 g, 0.05 mol) in 40 ml of dichloromethane. The temperature rises to 32° C. The mixture is refluxed for two hours. The reaction mixture is poured into 150 ml of water and is extracted with dichloromethane. The organic phases are washed with water and dried over sodium sulfate, and the solvent is then evaporated off. After purification by passing through a column of silica (eluent: 70/30 heptane/ethyl acetate), 12.2 g (70% yield) of cyano-N-[3-[1,3,3,3-tetramethyl-1-[(trimethylsilyl)oxy]disiloxanyl]propyl]acetamide are obtained in the form of a colorless oil, which is used without further purification in the following step.

후처리

  1. customrises to 32° C
  2. temperatureThe mixture is refluxed for two hours
  3. extractionis extracted with dichloromethane
  4. washThe organic phases are washed with water
  5. dry with materialdried over sodium sulfate
  6. customthe solvent is then evaporated off
  7. customAfter purification

출처 및 근거

ORD 기록
ord-3e13371d10094e938344fb47f79d8d8e
출처 데이터셋
uspto-grants-2008_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07439380B2

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