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

HRID 1983819Notes

Reaction equation

HRID 1983819 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 47.5%

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 56 at 280 g/Hr and the reactant 1-butanol (manufactured by Wako Pure Chemical Industries Ltd., Japan, industrial product) from supply line 57 at 1,332 g/Hr. The holding time in the reactor was 13 minutes. Reaction solution which accumulated in the reactor lower portion was circulated at 6,000 g/Hr by the circulation line 59 and the reboiler 60 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 68 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 63 and through the low boiling point component recovery line 65 for liquefaction at the condenser 66, and were thereby recovered from the liquid-phase recovery line 70 at 512 g/Hr. Low boiling point components were also recovered at 496 g/Hr from the reaction middle portion 62 via the liquid-phase recovery line 75. Furthermore, from the reactor lower portion 64, a dibutyltin alkoxide-containing component was recovered at 603 g/Hr from the extraction line 76. Analysis of the liquid recovered from the extraction line 76 showed that, using dibutyltin oxide as a reference, the liquid contained a dibutyltin alkoxide consisting of a yield of about 47.5% dibutyl-di(butyloxy)tin and 52.4% of 1,1,3,3-tetrabutyl-1,3-di(butyloxy)-distannoxane. Tributyltin butoxide had a yield of 0.021%. Meanwhile, the liquid recovered from the liquid-phase recovery lines 70 and 75 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 0.00081 mol/Hr calculated from expression (16).

Workup

  1. customprepared in the same manner as in Example 12 from supply line 56 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 70 at 512 g/Hr
  6. customwere also recovered at 496 g/Hr from the reaction middle portion 62 via the liquid-phase recovery line 75
  7. additionFurthermore, from the reactor lower portion 64, a dibutyltin alkoxide-containing component
  8. customwas recovered at 603 g/Hr from the extraction line 76
  9. customAnalysis of the liquid recovered from the extraction line 76

Sources & evidence

ORD record
ord-1f1c2922b20143628f30d54e27cab0c4
Source dataset
uspto-grants-2009_06
Patent number
US07541482B2

Reaction notes

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