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1,1,3,3-Tetrabutyl-1,3-diisothiocyanatodistannoxane → HCID 53691823, 화합물

HRID 483652
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HRID 483652 반응식
[Si:1]([O:18][CH2:19][CH2:20][CH2:21][CH2:22][CH:23]=[C:24]([F:33])[CH2:25][O:26]C1CCCCO1)([C:14]([CH3:17])([CH3:16])[CH3:15])([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C([Sn](CCCC)(N=C=S)O[Sn](CCCC)(CCCC)N=C=S)CCC>CO>[Si:1]([O:18][CH2:19][CH2:20][CH2:21][CH2:22][CH:23]=[C:24]([F:33])[CH2:25][OH:26])([C:14]([CH3:17])([CH3:15])[CH3:16])([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
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참가 물질

4

반응물 2

HCID 166879751,1,3,3-Tetrabutyl-1,3-diisothiocyanatodistannoxaneHCID 53929479HCID 53929479, 화합물

생성물 1

HCID 53691823HCID 53691823, 화합물수율 92%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

The tetrahydropyranyl derivative prepared in 3C (2.26 g, 4.8 mmoles) was dissolved in methanol. Tetrabutyl-1,3-diisothiocyanatodistannoxane (30 mg) was added and the mixture was refluxed for 24 hrs. Methanol was evaporated under reduced pressure. The residue was dissolved in ether and washed with water. The organic layer was dried over sodium sulfate, filtered and concentrated under reduced pressure. Flash chromatography on silicagel and elution with a 2:8 mixture of hexane and ethyl acetate afforded the alcohol as an oil (1.65 g, 92%).

후처리

  1. temperaturethe mixture was refluxed for 24 hrs
  2. customMethanol was evaporated under reduced pressure
  3. dissolutionThe residue was dissolved in ether
  4. washwashed with water
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. washFlash chromatography on silicagel and elution
  9. additionwith a 2:8 mixture of hexane and ethyl acetate

출처 및 근거

ORD 기록
ord-3cd2a0094a404788ac07294eb72aadac
출처 데이터셋
uspto-grants-1993_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05225429

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