Water → 1-Dimethylamino-2-Propyl Tributylstannyl Ether

HRID 65560

반응식

HRID 65560 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][CH:31](O)[CH3:32].O>C1C=CC=CC=1>[CH2:24]([Sn:15]([O:14][CH:31]([CH3:32])[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 962WaterHCID 37511DimepranolHCID 16682746Bis(tributyltin) oxide

생성물 1

HCID 227570361-Dimethylamino-2-Propyl Tributylstannyl Ether

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

1-Dimethylamino-2-Propyl Tributylstannyl Ether is prepared from 89.4 gm (0.15 mole) bis(tributyltin) oxide and 30.9 gm (0.3 mole) 1-dimethylamino-2-propanol in 200 ml benzene. This is stirred and heated to reflux in a system that contains a Dean-Starke tube. After refluxing 23 hours a total of 2.6 ml of water (theory 2.7 ml) had collected in the Dean-Starke tube. The solvent is stripped off on a rotating evaporator to provide 111.0 gm of yellow liquid. This is fractionated at reduced pressure with collection at 167°-175° C. at 0.5 mm of 63.4 gm of straw colored liquid. (Percent yield - 54). Infrared spectral analysis shows this liquid to be the desired ether.

후처리

  1. temperatureheated
  2. temperatureto reflux in a system that
  3. customhad collected in the Dean-Starke tube
  4. customThe solvent is stripped off on a rotating evaporator

출처 및 근거

ORD 기록
ord-4d932d6479674cca98ab916ec54b4a99
출처 데이터셋
uspto-grants-1978_12
특허 번호
US04128429

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