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

HRID 1983823Notes

Reaction equation

HRID 1983823 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 74.2%

Reagents, catalysts & solvents 1

HCID 2631-ButanolSolvent

Conditions

Temperature
141 °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 214 at 280 g/Hr and the reactant 1-butanol (manufactured by Wako Pure Chemical Industries Ltd., Japan, industrial product) from supply line 215 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 217 and the reboiler 218 while heating at a temperature of about 141° C. Low boiling point components flowed from the reactor upper portion 221 and through the low boiling point component recovery line 223 for liquefaction at the condenser 224, and were thereby recovered at 2,000 g/Hr. The organic layer and the water later were slowly separated at the separator 225. The organic layer in the separator 225, i.e. 1-butanol, was returned to the reactor upper portion 221 at 1,994 g/Hr via the organic layer circulation line 228, and the lower layer, which contained a high concentration of water, was recovered at 6 g/Hr from the water layer recovery line 229. From the reactor lower portion 222, the dibutyltin alkoxide-containing component was recovered at 1,604 g/Hr from the extraction line 230. The liquid temperature inside the reactor was 140° C., and the pressure of the back pressure valve 226 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. Analysis of the liquid recovered from the extraction line 230 showed that, using dibutyltin oxide as a reference, the liquid contained a dibutyltin alkoxide consisting of a yield of about 74.2% of dibutyl-di(butyloxy)tin and 25.7% of 1,1,3,3-tetrabutyl-1,3-di(butyloxy)-distannoxane. Tributyltin butoxide had a yield of 0.015%. Meanwhile, the liquid recovered from the water layer recovery line 229 was transparent and had a 90% by weight moisture content. The dehydration rate in the column reactor was 0.33 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 214 at 280 g/Hr
  2. customReaction solution which
  3. customwere thereby recovered at 2,000 g/Hr
  4. customThe organic layer and the water later were slowly separated at the separator 225
  5. concentrationa high concentration of water
  6. customwas recovered at 6 g/Hr from the water layer recovery line 229
  7. additionFrom the reactor lower portion 222, the dibutyltin alkoxide-containing component
  8. customwas recovered at 1,604 g/Hr from the extraction line 230
  9. customwas 140° C.
  10. waitContinuous supply was continued in this state for 10 hours
  11. customAnalysis of the liquid recovered from the extraction line 230

Sources & evidence

ORD record
ord-83fdd4a8e1054ca4b4b394d8fb0d1fda
Source dataset
uspto-grants-2009_06
Patent number
US07541482B2

Reaction notes

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