Water → N,N,N-Trimethyl-1-adamantylammonium hydroxide

HRID 2201605노트

반응식

HRID 2201605 반응식
C[O:2]C(=O)[O-].[C:6]12([N+:16]([CH3:19])([CH3:18])[CH3:17])[CH2:15][CH:10]3[CH2:11][CH:12]([CH2:14][CH:8]([CH2:9]3)[CH2:7]1)[CH2:13]2.O.[OH-].[Ca+2].[OH-]>CO>[OH-:2].[C:6]12([N+:16]([CH3:19])([CH3:18])[CH3:17])[CH2:13][CH:12]3[CH2:11][CH:10]([CH2:9][CH:8]([CH2:14]3)[CH2:7]1)[CH2:15]2

참가 물질

5

반응물 3

HCID 962WaterHCID 6093208Calcium HydroxideHCID 67399232HCID 67399232, 화합물

생성물 1

HCID 14475644N,N,N-Trimethyl-1-adamantylammonium hydroxide

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
10 °C

실험 절차

Adamantyltrimethylammonium methylcarbonate (383 g, 1.42 mol) is added to water (1000 mL), followed by addition of calcium hydroxide (148 g, 2.0 mol). This addition is exothermic. The reaction mixture is then heated to reflux and the methanol produced is slowly distilled off until the vapor temperature is constant. The reaction mixture is then cooled slowly to 10° C. and the precipitated calcium carbonate and excess calcium hydroxide are filtered off on a Nutsche filter. The filter cake is washed with water (200 mL) and both the mother and wash filtrates are combined. The 1-adamantyltrimethylammonium hydroxide product yield is 1284 grams of solution with assay 20.2% w/w.

후처리

  1. additionThis addition
  2. temperatureThe reaction mixture is then heated
  3. temperatureto reflux
  4. distillationis slowly distilled off until the vapor temperature
  5. filtrationthe precipitated calcium carbonate and excess calcium hydroxide are filtered off on a Nutsche
  6. filtrationfilter
  7. washThe filter cake is washed with water (200 mL)
  8. washboth the mother and wash filtrates

출처 및 근거

ORD 기록
ord-d07b2dc5c5f141c4af169c13fa9597b7
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09365490B2

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