Sodium Carbonate → Tris(tris(trimethylsiloxy)silylpropyl)amine

HRID 1478939ノート

反応式

HRID 1478939 の反応式
I[CH2:2][CH2:3][CH2:4][Si:5]([O:16][Si:17]([CH3:20])([CH3:19])[CH3:18])([O:11][Si:12]([CH3:15])([CH3:14])[CH3:13])[O:6][Si:7]([CH3:10])([CH3:9])[CH3:8].[NH2:21][CH2:22][CH2:23][CH2:24][Si:25]([O:36][Si:37]([CH3:40])([CH3:39])[CH3:38])([O:31][Si:32]([CH3:35])([CH3:34])[CH3:33])[O:26][Si:27]([CH3:30])([CH3:29])[CH3:28].C(=O)([O-])[O-].[Na+].[Na+]>CC(N(C)C)=O>[CH3:8][Si:7]([CH3:10])([CH3:9])[O:6][Si:5]([CH2:4][CH2:3][CH2:2][N:21]([CH2:2][CH2:3][CH2:4][Si:5]([O:16][Si:17]([CH3:19])([CH3:18])[CH3:20])([O:11][Si:12]([CH3:15])([CH3:14])[CH3:13])[O:6][Si:7]([CH3:8])([CH3:9])[CH3:10])[CH2:22][CH2:23][CH2:24][Si:25]([O:36][Si:37]([CH3:39])([CH3:38])[CH3:40])([O:26][Si:27]([CH3:28])([CH3:29])[CH3:30])[O:31][Si:32]([CH3:35])([CH3:34])[CH3:33])([O:16][Si:17]([CH3:20])([CH3:19])[CH3:18])[O:11][Si:12]([CH3:15])([CH3:14])[CH3:13]

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 2756547(3-Aminopropyl)tris(trimethylsiloxy)silaneHCID 223256933-Iodopropyl-tris(trimethylsiloxy)silane

生成物 1

HCID 86670505Tris(tris(trimethylsiloxy)silylpropyl)amine

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

反応条件

温度
80 °C

実験手順

14.3 g of 3-iodopropyltris(trimethylsiloxy)silane (28), 5.7 g of 3-aminopropyltris(trimethyl-siloxy)silane and 9.6 g of sodium carbonate are added to 50 ml dimethylacetamide and stirred for 15 hours at 80° C. The dimethylacetamide is then evaporated and the residue taken up in methylene chloride. The organic phase is washed with water, dried and evaporated. The product is purified by column chromatography on silica gel to give 7 g of a slightly yellowish oil of formula (30); 1H-NMR (ppm, CDCl3): 2.21 6H t, 1.38 6H txt, 0.28 6H t, 0 81H s.

後処理

  1. customThe dimethylacetamide is then evaporated
  2. washThe organic phase is washed with water
  3. customdried
  4. customevaporated
  5. customThe product is purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-8f5669107d6e42f5a259c26cffdf9dd8
出典データセット
uspto-grants-2016_08
特許番号
US09403987B2

反応ノート

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