Water → 2-Dimethylamino-2-Methyl-1-Propyl Tributylstannyl Ether

HRID 65557

反応式

HRID 65557 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]([CH3:35])[C:30]([CH3:34])([CH3:33])[CH2:31]O.O>C1C=CC=CC=1>[CH2:24]([Sn:15]([O:14][CH2:31][C:30]([N:29]([CH3:35])[CH3:28])([CH3:34])[CH3:33])([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 234352-(Dimethylamino)-2-methylpropanolHCID 16682746Bis(tributyltin) oxide

生成物 1

HCID 227570382-Dimethylamino-2-Methyl-1-Propyl Tributylstannyl Ether

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

2-Dimethylamino-2-Methyl-1-Propyl Tributylstannyl Ether is prepared from 59.6 gm (0.1 mole) bis(tributyltin) oxide and 23.4 gm (0.2 mole) 2-dimethylamino-2-methyl-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 water began to collect in the Dean-Starke tube and after 46 hours only 1.6 ml of water (theory 1.8 ml) had collected. Solvent is stripped off on a rotating evaporator to provide 78.3 gm of straw colored liquid. This is fractionated at reduced pressure to collect the desired product, 52.7 gm of water-white liquid (Percent yield - 65), at 132°-137° C. at 0.5 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 and after 46 hours only 1.6 ml of water (theory 1.8 ml)
  4. customhad collected
  5. customSolvent is stripped off on a rotating evaporator
  6. customto provide 78.3 gm of straw colored liquid
  7. customto collect the desired product, 52.7 gm of water-white liquid (Percent yield - 65)
  8. customat 132°-137° C.

出典と根拠

ORDレコード
ord-1196f53696f64bde99386c13c8232522
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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