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

HRID 1983818Notes

Reaction equation

HRID 1983818 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 46.3%

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 41 at 280 g/Hr and the reactant 1-butanol (manufactured by Wako Pure Chemical Industries Ltd., Japan, industrial product) from supply line 42 at 1,330 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 44 and the reboiler 45 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 52 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 47 and through the low boiling point component recovery line 49 for liquefaction at the condenser 50, and were thereby recovered from the liquid-phase recovery line 54 at 1,006 g/Hr. Furthermore, from the reactor lower portion 48, a dibutyltin alkoxide-containing component was recovered at 604 g/Hr from the extraction line 55. Analysis of the liquid recovered from the extraction line 55 showed that, using dibutyltin oxide as a reference, the liquid contained a dibutyltin alkoxide consisting of a yield of about 46.3% dibutyl-di(butyloxy)tin and 53.6% 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 54 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 41 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 54 at 1,006 g/Hr
  6. additionFurthermore, from the reactor lower portion 48, a dibutyltin alkoxide-containing component
  7. customwas recovered at 604 g/Hr from the extraction line 55
  8. customAnalysis of the liquid recovered from the extraction line 55

Sources & evidence

ORD record
ord-5aece3120ff5493ab2b3d01a13fb1369
Source dataset
uspto-grants-2009_06
Patent number
US07541482B2

Reaction notes

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