Dibutyltin oxide → Dibutyltin diethylmalonate

HRID 979273

반응식

HRID 979273 반응식
[CH2:1]([Sn:5](=O)[CH2:6][CH2:7][CH2:8][CH3:9])[CH2:2][CH2:3][CH3:4].[CH2:11]([C:13]([CH2:20][CH3:21])([C:17]([OH:19])=[O:18])[C:14]([OH:16])=[O:15])[CH3:12]>C1(C)C=CC=CC=1>[CH2:20]([C:13]([CH2:11][CH3:12])([C:17]([O-:19])=[O:18])[C:14]([O-:16])=[O:15])[CH3:21].[CH2:1]([Sn+2:5][CH2:6][CH2:7][CH2:8][CH3:9])[CH2:2][CH2:3][CH3:4]

참가 물질

4

반응물 2

HCID 61221Dibutyltin oxideHCID 68185Malonic acid, diethyl-

생성물 1

HCID 86741532Dibutyltin diethylmalonate수율 98%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of 300 grams of dibutyltin oxide, 193 grams of diethylmalonic acid, and 500 ml. of toluene was refluxed for 1 hour. There was collected 21 grams of water in a Dean Stock trap by azeotropic distillation. The reaction mixture was then filtered while hot and allowed to cool to ambient temperatures. Removal of the solvent in vacuo provided 460 grams (98% yield) of dibutyltin diethylmalonate as a white crystalline solid. The identity of the product was confirmed by NMR, IR and FD-MS analysis.

후처리

  1. customThere was collected 21 grams of water in a Dean Stock trap
  2. distillationby azeotropic distillation
  3. filtrationThe reaction mixture was then filtered while hot and
  4. temperatureto cool to ambient temperatures
  5. customRemoval of the solvent in vacuo

출처 및 근거

ORD 기록
ord-513107a2e36c4ceaa0523aa8baa07306
출처 데이터셋
uspto-grants-1987_05
특허 번호
US04667007

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