1-Butanol → Dibutoxydibutylstannane

HRID 1983816Notes

Reaction equation

HRID 1983816 reaction equation
C(=O)=O.C([Sn](CCCC)(OCCCC)[O:9][Sn:10]([CH2:20][CH2:21][CH2:22][CH3:23])([CH2:16][CH2:17][CH2:18][CH3:19])[O:11][CH2:12][CH2:13][CH2:14][CH3:15])CCC.[CH2:33](O)[CH2:34][CH2:35][CH3:36]>>[CH2:20]([Sn:10]([CH2:16][CH2:17][CH2:18][CH3:19])([O:9][CH2:33][CH2:34][CH2:35][CH3:36])[O:11][CH2:12][CH2:13][CH2:14][CH3:15])[CH2:21][CH2:22][CH3:23]

Participants

4

Reactant 3

HCID 2631-Butanol3×HCID 280Carbon DioxideHCID 167124431,3-Dibutoxy-1,1,3,3-tetrabutyldistannoxane2×

Product 1

HCID 16683936DibutoxydibutylstannaneYield 37.5%

Procedure

From the gas supply line 29, 1-butanol (manufactured by Wako Pure Chemical Industries Ltd., Japan, industrial product) was fed at 566 g/Hr and carbon dioxide was fed at 3 NL/Hr. All of the 1-butanol was vaporized by the heat exchanger 30 and fed to the reactor lower portion 33. A feed pump was used to start supplying the starting material 1,1,3,3-tetrabutyl-1,3-di(butyloxy)-distannoxane prepared in the same manner as in Example 12 from supply line 26 at 280 g/Hr and the reaction solution 1-butanol (manufactured by Wako Pure Chemical Industries Ltd., Japan, industrial product) from supply line 27 at 1,330 g/Hr. The holding time in the reactor was 13 minutes. The liquid temperature inside the reactor was 140° C., and the pressure of the back pressure valve 37 was adjusted to 0.096 MPa-G. Continuous supply was continued in this state for 10 hours, after which the system reached a steady state. Low boiling point components flowed from the reactor upper portion 32 and through the low boiling point component recovery line for liquefaction at the condenser 35, and were thereby recovered from the liquid-phase recovery line 39 at 1,006 g/Hr. Furthermore, from the reactor lower portion 33 a dibutyltin alkoxide-containing component was recovered at 1,170 g/Hr from the extraction line 40. Analysis of the liquid recovered from the generated product extraction line 40 showed that, using dibutyltin oxide as a reference, the liquid contained a dibutyltin alkoxide consisting of a yield of about 37.5% dibutyl-di(butyloxy)tin and 62.4% of 1,1,3,3-tetrabutyl-1,3-di(butyloxy)-distannoxane. Tributyltin butoxide had a yield of 0.022%. Meanwhile, the liquid recovered from the liquid-phase recovery line 39 was transparent and contained 2,200 ppm of moisture. The dehydration rate in the column reactor was 0.39 mol/Hr, which was greater than the value 0.0015 mol/Hr calculated from expression (16).

Workup

  1. customprepared in the same manner as in Example 12 from supply line 26 at 280 g/Hr
  2. customwas 140° C.
  3. waitContinuous supply was continued in this state for 10 hours
  4. customwere thereby recovered from the liquid-phase recovery line 39 at 1,006 g/Hr
  5. additionFurthermore, from the reactor lower portion 33 a dibutyltin alkoxide-containing component
  6. customwas recovered at 1,170 g/Hr from the extraction line 40
  7. customAnalysis of the liquid recovered from the generated product extraction line 40

Sources & evidence

ORD record
ord-54e5d5ee14e145aab5595d4b477474b0
Source dataset
uspto-grants-2009_06
Patent number
US07541482B2

Reaction notes

Loading…