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.[CH2:28]([N:32]([CH2:36][CH2:37][CH2:38][CH3:39])[CH2:33][CH2:34]O)[CH2:29][CH2:30][CH3:31].O>C1C=CC=CC=1>[CH2:24]([Sn:15]([O:14][CH2:34][CH2:33][N:32]([CH2:36][CH2:37][CH2:38][CH3:39])[CH2:28][CH2:29][CH2:30][CH3:31])([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
実験手順
N,N-Dibutylaminoethyl Tributylstannyl Ether is prepared from 59.6 gm (0.1 mole) bis(tributyltin) oxide and 34.6 gm (0.2 mole) N,N-dibutylethanolamine in 200 ml benzene. This is stirred and heated to reflux in a system that contains a Dean-Starke tube. After 30 minutes water began to collect in the Dean-Starke tube and after refluxing for a period of 22 hours a total of 1.8 ml of water (theory 1.8 ml) had collected. A rotating evaporator is used to remove the benzene and to provide 95.1 gm of red-orange liquid. This is fractionated at reduced pressure with collection at 163°-166° C. at 0.7 mm of 73.1 gm of yellow liquid (Percent yield - 79). Infrared spectral analysis shows this to be the desired ether.
後処理
- temperatureheated
- temperatureto reflux in a system that
- customto collect in the Dean-Starke tube
- temperatureafter refluxing for a period of 22 hours a total of 1.8 ml of water (theory 1.8 ml)
- customhad collected
- customA rotating evaporator
- customto remove the benzene
出典と根拠
- ORDレコード
- ord-76d8c9240e5b4ffb84253ad3175855bc
- 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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