Water → 2-(2-Pyridyl)ethyl Tributylstannyl Ether

HRID 65555

反応式

HRID 65555 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.O[CH2:29][CH2:30][C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][N:32]=1.O>C1C=CC=CC=1>[CH2:24]([Sn:15]([O:14][CH2:29][CH2:30][C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][N:32]=1)([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 962WaterHCID 76752-(2-Hydroxyethyl)pyridineHCID 16682746Bis(tributyltin) oxide

生成物 1

HCID 227570462-(2-Pyridyl)ethyl Tributylstannyl Ether

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

2-(2-Pyridyl)ethyl Tributylstannyl Ether is prepared from 59.6 gm (0.1 mole) of bis(tributyltin) oxide and 24.6 gm (0.2 mole) 2-(β-hydroxyethyl)pyridine 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 22 hours a total of 2.0 ml of water (theory 1.8 ml) had collected. This is evaporated on a rotating evaporator to provide 82.6 gm of straw colored liquid, which fractionated at reduced pressure. 66.4 gm. of a straw colored liquid are collected at 155°-158° C. at 0.5 mm. (Percent yield - 80.6). 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 22 hours a total of 2.0 ml of water (theory 1.8 ml)
  5. customhad collected
  6. customThis is evaporated on a rotating evaporator
  7. customto provide 82.6 gm of straw colored liquid, which
  8. customof a straw colored liquid are collected at 155°-158° C. at 0.5 mm

出典と根拠

ORDレコード
ord-5fcbd75c614143138fcabe0ae10ede7a
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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