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Tributyltin Chloride → HCID 13019239、化合物

HRID 596752
ノート
印刷プレビュー

反応式

HRID 596752 の反応式
[CH2:1]([Sn:5]([CH2:18][CH2:19][CH2:20][CH3:21])([CH:12]1CC[CH2:15][CH2:14][CH2:13]1)[CH:6]1[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1)[CH2:2][CH2:3][CH3:4].[CH:22]1([Mg]Cl)[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]1.[CH2:30]([Sn:34]([Cl:43])(CCCC)[CH2:35][CH2:36][CH2:37][CH3:38])[CH2:31][CH2:32][CH3:33].C([Sn](CCCC)(CCCC)C1CCCCC1)CCC>[Hg].CCCCC>[CH2:18]([Sn:5]([CH2:1][CH2:2][CH2:3][CH3:4])([CH2:12][CH2:13][CH2:14][CH3:15])[CH:6]1[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1)[CH2:19][CH2:20][CH3:21].[CH2:30]([Sn:34]([Cl:43])([CH2:35][CH2:36][CH2:37][CH3:38])[CH:22]1[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]1)[CH2:31][CH2:32][CH3:33]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 15096Tributyltin ChlorideHCID 534724Stannane, cyclohexyltributyl-HCID 11101403HCID 11101403、化合物HCID 178478990HCID 178478990、化合物

生成物 2

HCID 534724Stannane, cyclohexyltributyl-HCID 13019239HCID 13019239、化合物収率 93.2%

試薬・触媒・溶媒 2

HCID 23931Mercury触媒HCID 8003Pentane溶媒2 回

反応条件

温度
36 °C

実験手順

Tributylcyclohexyl stannane was prepared using a procedure similar to that described in Example 1 for dibutyldicyclohexyl stannane, with the exception that a 25% molar excess of cyclohexylmagnesium chloride was reacted with tributyltin chloride. The boiling point of the product was 123° C. under a pressure of 0.7 mm. of mercury. A solution containing 37.3 grams (0.1 mole) of tributylcyclohexyl stannane in 50 cc. of pentane was placed in a reaction vessel equipped with a thermometer, mechanically driven stirrer, addition funnel, watercooled reflux condenser, and nitrogen inlet. To this was gradually added over a 25 minute period a solution containing 6.1 grams (0.1 mole) of stannic chloride in 50 cc. of pentane. During the addition, the temperature of the reaction mixture rose from 25° to 36° C. and the initially clear, colorless solution turned cloudy and yellow. After heating the solution to reflux temperature (36° C.) for 15 minutes, it was allowed to cool to ambient temperature. The product was extracted using 55 cc. of a 1.2 molar aqueous hydrochloric acid solution. The resultant two-phase mixture was transferred to a separatory funnel and the lower aqueous layer drawn off and discarded. The organic layer was extracted with two-50 cc. portions of 1.2 molar aqueous hydrochloric acid solution followed by two-50 cc. portions of water. The organic layer was then dried over anhydrous sodium sulfate, which was subsequently removed by filtration. The filtrate was concentrated using a rotary evaporator to yield 32.8 grams (93.2% yield) of dibutylcyclohexyltin chloride, a hazy, colorless liquid exhibiting an index of refraction (nD25) of 1.5079. The crude product was distilled under reduced pressure to yield 29.3 grams of dibutylcyclohexyltin chloride boiling between 139° and 140° C. at a pressure between 0.8 and 0.9 millimeter of mercury.

後処理

  1. customwas 123° C. under a pressure of 0.7 mm
  2. customequipped with a thermometer, mechanically driven stirrer, addition funnel
  3. temperaturewatercooled reflux condenser, and nitrogen inlet
  4. additionTo this was gradually added over a 25 minute period a solution
  5. additionDuring the addition
  6. customrose from 25° to 36° C.
  7. temperatureAfter heating the solution
  8. temperatureto cool to ambient temperature
  9. extractionThe product was extracted
  10. customThe resultant two-phase mixture was transferred to a separatory funnel
  11. extractionThe organic layer was extracted with two-50 cc
  12. dry with materialThe organic layer was then dried over anhydrous sodium sulfate, which
  13. customwas subsequently removed by filtration
  14. concentrationThe filtrate was concentrated
  15. customa rotary evaporator

出典と根拠

ORDレコード
ord-d646bbc6b911400a8e8714579744737d
出典データセット
uspto-grants-1977_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04012347

反応ノート

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