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Dibutyltin oxide → HCID 59487992, 화합물

HRID 1881387
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HRID 1881387 반응식
[CH2:1]([Sn:5](=[O:10])[CH2:6][CH2:7][CH2:8][CH3:9])[CH2:2][CH2:3][CH3:4].[OH:11][C:12]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)([CH2:21]O)[C:13]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)=[O:14]>C1(C)C=CC=CC=1>[CH2:1]([Sn:5]1([CH2:6][CH2:7][CH2:8][CH3:9])[O:11][C:12]([C:13](=[O:14])[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[CH2:21][O:10]1)[CH2:2][CH2:3][CH3:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 61221Dibutyltin oxideHCID 858062,3-Dihydroxy-1,2-diphenylpropan-1-one

생성물 1

HCID 59487992HCID 59487992, 화합물수율 40.7%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

In a 50 ml dry three-neck-flask 2.1 g (8.3 mmol) of dibutyltin oxide, 2.0 g (8.3 mmol) of 2,3-dihydroxy-1,2-diphenyl-propan-1-one [prepared according to H. J. Hageman, Macromolekulare Chemie, Rapid Communications (1981), 2(8), 517-521] and 20 ml of toluene are heated to reflux under argon flow. A small amount of water is distilled off the clear solution. According to the 1H-NMR-spectrum the conversion is complete after 2 h. The solution is concentrated and the crude product (4.0 g) is recrystallized from 15 ml of cyclohexane. The white crystals (2.3 g) are recrystallized from 10 ml of heptane and 3 ml of cyclohexane. 1.6 g of the title product is obtained as a white powder melting at 140-145° C. The structure is further confirmed by 1H-NMR and 13C-NMR-spectra.

후처리

  1. temperatureare heated
  2. temperatureto reflux under argon flow
  3. distillationA small amount of water is distilled off the clear solution
  4. concentrationThe solution is concentrated
  5. customthe crude product (4.0 g) is recrystallized from 15 ml of cyclohexane
  6. customThe white crystals (2.3 g) are recrystallized from 10 ml of heptane and 3 ml of cyclohexane

출처 및 근거

ORD 기록
ord-5cf62fc42ce24ef3b350987d64d9d44d
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08318830B2

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