(3-Aminopropyl)triethoxysilane → 4-(3-Triethoxysilylpropyl)Semicarbazide

HRID 236632

반응식

HRID 236632 반응식
[NH2:1][CH2:2][CH2:3][CH2:4][Si:5]([O:12][CH2:13][CH3:14])([O:9][CH2:10][CH3:11])[O:6][CH2:7][CH3:8].[NH:15]([C:17](OC)=[O:18])[NH2:16]>CO.C(O)C>[CH2:10]([O:9][Si:5]([O:12][CH2:13][CH3:14])([O:6][CH2:7][CH3:8])[CH2:4][CH2:3][CH2:2][NH:1][C:17](=[O:18])[NH:15][NH2:16])[CH3:11]

참가 물질

4

반응물 2

HCID 13521(3-Aminopropyl)triethoxysilaneHCID 80519Methyl carbazate

생성물 1

HCID 202164984-(3-Triethoxysilylpropyl)Semicarbazide

시약·촉매·용매 1

HCID 18681192Ethanol, mixt. with methanol용매

실험 절차

A mixture of 44.2 g (0.20 mole) 3-aminopropyltriethoxysilane and 18.0 g (0.20 mole) methyl hydrazinocarboxylate under nitrogen was gradually heated to 150° C. with a slow distillation of the evolved methanol/ethanol from the reaction. After 2 hours at 150° C., 9.1 g. of distillate had been collected, and the reaction mass was cooled to ambient. The pale yellow oil was decanted from the small amount of white solid; yield 51 g (91%). IR (neat) 3320, 1640 (br), 1540 (br), 1070 (br), 940, 790 cm-1. NMR (CDCl3) 0.4-1.0 (m; 2H), 1.2 (t; 9H), 1.3-2.0 (m; 2H), 2.9-3.5 (m; 2H), 3.5-4.1 (m; 8H), 6.3 (br; 2H) ppm.

후처리

  1. distillationof distillate had been collected
  2. temperaturethe reaction mass was cooled
  3. customThe pale yellow oil was decanted from the small amount of white solid

출처 및 근거

ORD 기록
ord-4916c91e18e84e1eb2f1fcf43cd6af01
출처 데이터셋
uspto-grants-1987_02
특허 번호
US04645846

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