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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Water → HCID 21107845、化合物

HRID 2116804
ノート
印刷プレビュー

反応式

HRID 2116804 の反応式
[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]
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 4

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

生成物 1

HCID 21107845HCID 21107845、化合物収率 70.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3e13371d10094e938344fb47f79d8d8e
出典データセット
uspto-grants-2008_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07439380B2

反応ノート

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