1,3-Dibutoxy-1,1,3,3-tetrabutyldistannoxane → Dibutoxydibutylstannane

HRID 1983820Notes

Reaction equation

HRID 1983820 reaction equation
C([Sn](CCCC)(OCCCC)[O:6][Sn:7]([CH2:17][CH2:18][CH2:19][CH3:20])([CH2:13][CH2:14][CH2:15][CH3:16])[O:8][CH2:9][CH2:10][CH2:11][CH3:12])CCC>C(O)CCC>[CH2:17]([Sn:7]([CH2:13][CH2:14][CH2:15][CH3:16])([O:6][CH2:9][CH2:10][CH2:11][CH3:12])[O:8][CH2:9][CH2:10][CH2:11][CH3:12])[CH2:18][CH2:19][CH3:20]

Participants

3

Reactant 1

HCID 167124431,3-Dibutoxy-1,1,3,3-tetrabutyldistannoxane2×

Product 1

HCID 16683936DibutoxydibutylstannaneYield 47%

Reagents, catalysts & solvents 1

HCID 2631-ButanolSolvent

Conditions

Temperature
140 °C

Procedure

A feed pump was used to start feeding 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 77 at 280 g/Hr and the reactant 1-butanol (manufactured by Wako Pure Chemical Industries Ltd., Japan, industrial product) from supply line 78 at 1,330 g/Hr. The holding time in the reactor was 6 minutes. Reaction solution which accumulated in the reactor lower portion was circulated at 6,000 g/Hr by the circulation line 80 and the reboiler 81 while heating at a temperature of about 140° C. The liquid temperature inside the reactor was 140° C., and the pressure of the back pressure valve 89 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 84 and through the low boiling point component recovery line 86 for liquefaction at the condenser 87, and were thereby recovered from the liquid-phase recovery line 91 at 1,031 g/Hr. Furthermore, from the reactor lower portion 85, a dibutyltin alkoxide-containing component was recovered at 602 g/Hr from the extraction line 92. Analysis of the recovered liquid showed that, using dibutyltin oxide as a reference, the liquid contained a dibutyltin alkoxide consisting of a yield of about 47.0% dibutyl-di(butyloxy)tin and 52.9% of 1,1,3,3-tetrabutyl-1,3-di(butyloxy)-distannoxane. Tributyltin butoxide had a yield of 0.012%. Meanwhile, the liquid recovered from the liquid-phase recovery line 91 was transparent and contained 2,200 ppm of moisture. The dehydration rate in the column reactor was 0.21 mol/Hr, which was greater than the value 0.00037 mol/Hr calculated from expression (16).

Workup

  1. customprepared in the same manner as in Example 12 from supply line 77 at 280 g/Hr
  2. customReaction solution which
  3. customwas 140° C.
  4. waitContinuous supply was continued in this state for 10 hours
  5. customwere thereby recovered from the liquid-phase recovery line 91 at 1,031 g/Hr
  6. additionFurthermore, from the reactor lower portion 85, a dibutyltin alkoxide-containing component
  7. customwas recovered at 602 g/Hr from the extraction line 92

Sources & evidence

ORD record
ord-41ef254a02cf4291be65bbf86d22f6e4
Source dataset
uspto-grants-2009_06
Patent number
US07541482B2

Reaction notes

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