1-Butanol → Dibutoxydibutylstannane

HRID 1983815Notes

Reaction equation

HRID 1983815 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 41.3%

Procedure

From the gas supply line 29, 1-butanol (manufactured by Wako Pure Chemical Industries Ltd., Japan, industrial product) was fed at 399 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 feeding the starting material 1,1,3,3-tetrabutyl-1,3-di(butyloxy)-distannoxane from supply line 26 at 210 g/Hr and the reaction solution 1-butanol (manufactured by Wako Pure Chemical Industries Ltd., Japan, industrial product) from supply line 27 at 951 g/Hr. The holding time in the reactor was 30 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 753 g/Hr. Furthermore, from the reactor lower portion 33, a dibutyltin alkoxide-containing component was recovered at 807 g/Hr from the extraction line 40. Analysis of the recovered liquid showed that, using dibutyltin oxide as a reference, the liquid contained dibutyltin alkoxide consisting of a yield of about 41.3% dibutyl-di(butyloxy)tin and 58.7% of 1,1,3,3-tetrabutyl-1,3-di(butyloxy)-distannoxane. Tributyltin butoxide had a yield of 0.04%. Meanwhile, the liquid recovered from the liquid-phase recovery line 39 was transparent and contained 2,500 ppm of moisture. The dehydration rate in the column reactor was 0.144 mol/Hr, which was greater than the value 0.0015 mol/Hr calculated from expression (16).

Workup

  1. customwas 140° C.
  2. waitContinuous supply was continued in this state for 10 hours
  3. customwere thereby recovered from the liquid-phase recovery line 39 at 753 g/Hr
  4. additionFurthermore, from the reactor lower portion 33, a dibutyltin alkoxide-containing component
  5. customwas recovered at 807 g/Hr from the extraction line 40

Sources & evidence

ORD record
ord-c2af2c8c8bd946a6b0b8225b5fe08e66
Source dataset
uspto-grants-2009_06
Patent number
US07541482B2

Reaction notes

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