1-Butanol → Bis(dibutylchlorotin) Phosphate

HRID 1106283노트

반응식

HRID 1106283 반응식
[CH2:1]([Sn:5](Cl)([Cl:10])[CH2:6][CH2:7][CH2:8][CH3:9])[CH2:2][CH2:3][CH3:4].C(O)CCC.O.O.[P:19]([O-:23])([O-:22])([O-:21])=[O:20].[Na+].[Na+].[Na+]>O>[P:19]([OH:23])([O-:22])([O-:21])=[O:20].[CH2:1]([Sn+:5]([CH2:6][CH2:7][CH2:8][CH3:9])[Cl:10])[CH2:2][CH2:3][CH3:4].[CH2:1]([Sn+:5]([CH2:6][CH2:7][CH2:8][CH3:9])[Cl:10])[CH2:2][CH2:3][CH3:4]

참가 물질

5

반응물 3

HCID 2631-ButanolHCID 12688Dibutyltin dichlorideHCID 18623014Trisodium;phosphate;dihydrate

생성물 1

HCID 20553860Bis(dibutylchlorotin) Phosphate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A glass reactor was charged with 91.1 g (0.3 mole) dibutyltin dichloride, 200 cc n-butanol, 50 cc water and 27.3 g (0.15 mole) dibasic sodium phosphate dihydrate. The resultant mixture was heated under a nitrogen atmosphere and the water removed by azeotropic distillation until the vapor temperature reached 117° C. The reaction mixture was then filtered and the liquid phase was concentrated under reduced pressure. The liquid residue solidified upon standing and weighed 83 g. The product was found to contain 34.60% tin, 11.18% chlorine and 4.42% phosphorus. The calculated values for these elements in the expected product are 37.53% tin, 11.21% chlorine and 4.90% phosphorus.

후처리

  1. customthe water removed by azeotropic distillation until the vapor temperature
  2. customreached 117° C
  3. filtrationThe reaction mixture was then filtered
  4. concentrationthe liquid phase was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-7624373b99824b889b3cf0d978fd40db
출처 데이터셋
uspto-grants-1982_01
특허 번호
US04312959

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