Water → 3-Dimethylamino-1-Propyl Tributylstannyl Ether

HRID 65556

반응식

HRID 65556 반응식
CCCC[Sn]([O:14][Sn:15]([CH2:24][CH2:25][CH2:26][CH3:27])([CH2:20][CH2:21][CH2:22][CH3:23])[CH2:16][CH2:17][CH2:18][CH3:19])(CCCC)CCCC.[CH3:28][N:29]([CH3:34])[CH2:30][CH2:31][CH2:32]O.O>C1C=CC=CC=1>[CH2:24]([Sn:15]([O:14][CH2:32][CH2:31][CH2:30][N:29]([CH3:34])[CH3:28])([CH2:16][CH2:17][CH2:18][CH3:19])[CH2:20][CH2:21][CH2:22][CH3:23])[CH2:25][CH2:26][CH3:27]

참가 물질

5

반응물 3

HCID 962Water2회HCID 766463-(Dimethylamino)-1-propanolHCID 16682746Bis(tributyltin) oxide

생성물 1

HCID 227570483-Dimethylamino-1-Propyl Tributylstannyl Ether

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

3-Dimethylamino-1-Propyl Tributylstannyl Ether is prepared from 59.6 gm (0.1 mole) bis(tributyltin) oxide and 20.6 gm (0.2 mole) 3-dimethylamino-1-propanol in 200 ml benzene. This is stirred and heated to reflux in a system that contains a Dean-Starke tube. After 30 minutes refluxing water began to collect in the Dean-Starke tube and after refluxing for 22 hours a total of 1.9 ml of water (theory 1.8 ml) had collected. The benzene is stripped off on a rotating evaporator to provide 77.1 gm of straw colored liquid. This is fractionated at reduced pressure, with 53.0 gm water-white liquid (Percent yield - 67.6) being collected at 135°-139° C. at 0.7 mm. Infrared spectral analysis shows this to be the desired ether.

후처리

  1. temperatureheated
  2. temperatureto reflux in a system that
  3. customto collect in the Dean-Starke tube
  4. temperatureafter refluxing for 22 hours a total of 1.9 ml of water (theory 1.8 ml)
  5. customhad collected
  6. customThe benzene is stripped off on a rotating evaporator
  7. customto provide 77.1 gm of straw colored liquid
  8. custombeing collected at 135°-139° C. at 0.7 mm

출처 및 근거

ORD 기록
ord-c4e215baf26540d69a92d44973124645
출처 데이터셋
uspto-grants-1978_12
특허 번호
US04128429

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