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Methanol → HCID 131713684, 화합물

HRID 1632594
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HRID 1632594 반응식
[CH3:1][O:2][CH:3]([O:6][CH3:7])[CH2:4][SH:5].[C:8]([O-:11])([O-])=[O:9].[K+].[K+].C([O:17][C:18](=[CH2:22])[C:19](=O)[CH3:20])(=O)C.[CH3:23]O>>[CH3:1][O:2][CH:3]([O:6][CH3:7])[CH:4]([S:5][CH2:20][CH2:19][C:18](=[O:17])[CH3:22])[O:11][C:8](=[O:9])[CH3:23]
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참가 물질

5

반응물 4

HCID 887MethanolHCID 11430Potassium CarbonateHCID 11073438HCID 11073438, 화합물HCID 148182602,2-Dimethoxyethane-1-thiol

생성물 1

HCID 131713684HCID 131713684, 화합물

실험 절차

To a solution of 15 g. (0.123 mol) of 2-mercaptoacetaldehyde dimethylacetal in 150 ml. of methanol was added 225 mg. of K2CO3 and 15.8 g. (0.123 mol) of 3-acetoxy-3-buten-2-one. After 2 hours at ambient temperature, the solvent was removed in vacuo, the oily residue dissolved in ether, washed with water and dried over Na2SO4. Filtration and removal of solvent in vacuo afforded 24.9 g. (81%) of the crude product: 1H-NMR (CDCl3) delta 2.15 (s, 3), 2.19 (s, 3), 2.74 (d, 2, J=5.4 Hz), 3.03 (m, 2), 3.34 (s, 6), 4.50 (t, 1, J=5.4 Hz), 5.22 (d of d, 1); 13C-NMR (CDCl3) delta 203.5 (s), 169.7 (s), 104.6 (d), 77.5 (d), 53.5 (q), 53.3 (g), 34.5 (d), 32.4 (t), 26.6 (q), 20.3 (q); mass spectrum (70 eV) m/e 250.0855 (parent, calcd. for C10H18O5S; 250.1134); IR (film) cm1 1747 (s), 1733 (s).

후처리

  1. customthe solvent was removed in vacuo
  2. dissolutionthe oily residue dissolved in ether
  3. washwashed with water
  4. dry with materialdried over Na2SO4
  5. filtrationFiltration and removal of solvent in vacuo
  6. customafforded 24.9 g

출처 및 근거

ORD 기록
ord-c62dc3baba584d66aa6c5a5d632147ea
출처 데이터셋
uspto-grants-1984_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04476312

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