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

HRID 1983817Notes

Reaction equation

HRID 1983817 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 44.4%

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 1,400 g/Hr. The holding time in the reactor was 24 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 were 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 1,010 g/Hr. Furthermore, from the reactor lower portion 48, a dibutyltin alkoxide-containing component was recovered at 670 g/Hr from the extraction line 55. 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 44.4% dibutyl-di(butyloxy)tin and 55.0% of 1,1,3,3-tetrabutyl-1,3-di(butyloxy)-distannoxane. Tributyltin butoxide had a yield of 0.05%. Meanwhile, the liquid recovered from the liquid-phase recovery line 54 was transparent and contained 2,300 ppm of moisture. The dehydration rate in the column reactor was 0.20 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 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 1,010 g/Hr
  6. additionFurthermore, from the reactor lower portion 48, a dibutyltin alkoxide-containing component
  7. customwas recovered at 670 g/Hr from the extraction line 55

Sources & evidence

ORD record
ord-f5c44c6fd46640cba7d4a3be9e8b92ff
Source dataset
uspto-grants-2009_06
Patent number
US07541482B2

Reaction notes

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