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

HRID 1478939노트

반응식

HRID 1478939 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 86670505Tris(tris(trimethylsiloxy)silylpropyl)amine

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

반응 조건

온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8f5669107d6e42f5a259c26cffdf9dd8
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09403987B2

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