Water → 3-Dimethylamino-1-Propyl Tributylstannyl Ether

HRID 65556

反応式

HRID 65556 の反応式
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]

参加物

5

反応物 3

HCID 962Water2 回HCID 766463-(Dimethylamino)-1-propanolHCID 16682746Bis(tributyltin) oxide

生成物 1

HCID 227570483-Dimethylamino-1-Propyl Tributylstannyl Ether

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c4e215baf26540d69a92d44973124645
出典データセット
uspto-grants-1978_12
特許番号
US04128429

関連ノート

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