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4-Methylbenzenethiol → (2R,3R,4S,5S,6R)-2-(acetoxymethyl)-6-(p-tolylthio)tetrahydro-2H-pyran-3,4,5-triyl triacetate

HRID 1862750
ノート
印刷プレビュー

反応式

HRID 1862750 の反応式
[C:1]([O:4][C@@H:5]([C@H:8]([C@@H:13]([C@@H:18]([CH2:23][O:24][C:25](=[O:27])[CH3:26])[O:19][C:20](=[O:22])[CH3:21])[O:14][C:15](=[O:17])[CH3:16])[O:9][C:10](=O)C)C=O)(=[O:3])[CH3:2].[CH3:28][C:29]1[CH:34]=[CH:33][C:32]([SH:35])=[CH:31][CH:30]=1.B(F)(F)F.CCOCC>C(Cl)Cl>[C:25]([O:24][C@H:23]1[C@@H:18]([O:19][C:20](=[O:22])[CH3:21])[C@H:13]([O:14][C:15](=[O:17])[CH3:16])[C@@H:8]([CH2:5][O:4][C:1](=[O:3])[CH3:2])[O:9][C@@H:10]1[S:35][C:32]1[CH:33]=[CH:34][C:29]([CH3:28])=[CH:30][CH:31]=1)(=[O:27])[CH3:26]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 78114-MethylbenzenethiolHCID 8000Boron trifluoride etherateHCID 11383716Mannose pentaacetate

生成物 1

HCID 11775389(2R,3R,4S,5S,6R)-2-(acetoxymethyl)-6-(p-tolylthio)tetrahydro-2H-pyran-3,4,5-triyl triacetate収率 87%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a mixture of D-mannose pentaacetate (16.0 g, 0.041 mol) and p-thiocresol (7.6 g, 0.0615 mol) in CH2Cl2 (200 mL), boron trifluoride diethyl etherate (6.8 mL, 0.0533 mol) was added. The mixture was stirred overnight. The reaction mixture was then diluted with CH2Cl2 (200 mL), washed with sat. NaHCO3 (2×120 mL) and water (100 mL). The organic layer was dried over Na2SO4. The solvent was removed, and the residue was purified by column chromotography on silia gel (hexanes/EtOAc 3:1) to give product (16.2 g, 87%) as a syrup: 1HNMR (500 MHz, CDCl3), δ 7.38 (d, J=8.0 Hz, 2H), 7.12 (d, J=8.0 Hz, 2H), 5.49 (dd, 1H, J=2.5, 1.5 Hz), 5.42 (d, 1H, J=1.0 Hz), 5.30-5.35 (m, 2H), 4.54-4.58 (m, 1H), 4.30 (dd, 1H, J=12.5, 6.0 Hz), 4.11 , (dd, 1H, J=12.0, 2.5 Hz), 2.33 (s, 3H), 2.15 (s, 3H), 2.08 (s, 3H), 2.06 (s, 3H), 2.02 (s, 3H); HRMS (M+Cs) calcd for C21H26O9SCs 587.0352, found 587.0331.

後処理

  1. additionwas added
  2. washwashed with sat. NaHCO3 (2×120 mL) and water (100 mL)
  3. dry with materialThe organic layer was dried over Na2SO4
  4. customThe solvent was removed
  5. customthe residue was purified by column chromotography on silia gel (hexanes/EtOAc 3:1)

出典と根拠

ORDレコード
ord-6bc9f2966c884d38a4b2214f0713ac19
出典データセット
uspto-grants-2003_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06538117B1

反応ノート

読み込み中…

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