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Chlorotrimethylsilane → HCID 86731802、化合物

HRID 1772582
ノート
印刷プレビュー

反応式

HRID 1772582 の反応式
[CH2:1]([O:4][CH2:5][CH2:6][NH2:7])[CH:2]=[CH2:3].[CH3:8][O:9][SiH:10]([O:13][CH3:14])[O:11][CH3:12].C(N(CC)CC)C.[CH3:22][Si:23]([CH3:26])([CH3:25])Cl>C([Si](C)(C)O[Si](C=C)(C)C)=C.[Pt].C1(C)C=CC=CC=1>[CH3:22][Si:23]([CH3:26])([CH3:25])[N:7]([Si:23]([CH3:26])([CH3:25])[CH3:22])[CH2:6][CH2:5][O:4][CH2:1][CH2:2][CH2:3][Si:10]([O:13][CH3:14])([O:11][CH3:12])[O:9][CH3:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 6397ChlorotrimethylsilaneHCID 8471TriethylamineHCID 17215TrimethoxysilaneHCID 2612732-(Prop-2-en-1-yloxy)ethan-1-amine

生成物 1

HCID 86731802HCID 86731802、化合物収率 86%

試薬・触媒・溶媒 2

HCID 10959889Platinum(0)-1,3-divinyl-1,1,3,3-tetramethyldisiloxane
触媒
HCID 1140Toluene溶媒

実験手順

After adding toluene (200 mL) to a round-bottom flask containing 2-(allyloxy)ethanamine (0.398 mol) and dissolving trimethoxysilane (0.398 mol), a commercially available platinum(0)-1,3-divinyl-1,1,3,3-tetramethyldisiloxane solution was added and the mixture was stirred for 24 hours. Upon completion of reaction, after removing the solvent through distillation under reduced pressure and extracting with water and diethyl ether, the product was dissolved in dichloromethane (200 mL). After adding triethylamine (1.0 mol) and trimethylchlorosilane (0.8 mol), the mixture was stirred for a day at room temperature. Upon completion of reaction, after removing the solvent through distillation under reduced pressure, 0.342 mol (yield: 86%) of the target compound was obtained by extracting with water and diethyl ether. 1H and 13C NMR spectroscopic data of the purified N,N-bis(trimethylsilyl)-2-(3-(trimethoxysilyl)propoxy)ethanamine are as follows.

後処理

  1. customUpon completion of reaction
  2. customafter removing the solvent
  3. distillationthrough distillation under reduced pressure
  4. extractionextracting with water and diethyl ether
  5. dissolutionthe product was dissolved in dichloromethane (200 mL)
  6. stirringthe mixture was stirred for a day at room temperature
  7. customUpon completion of reaction
  8. customafter removing the solvent
  9. distillationthrough distillation under reduced pressure

出典と根拠

ORDレコード
ord-f9137ce9facd44a19be7f5f6e1dc9e49
出典データセット
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09249276B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート