3,4-dihydro-2H-pyran → 2H-Pyran, tetrahydro-2-[(1-methyl-3-butynyl)oxy]-

HRID 872884

反応式

HRID 872884 の反応式
[CH3:1][CH:2]([OH:6])[CH2:3][C:4]#[CH:5].[O:7]1[CH:12]=[CH:11][CH2:10][CH2:9][CH2:8]1.N1C=CC=CC=1.C1(C)C=CC(S(O)(=O)=O)=CC=1>C(Cl)Cl>[CH3:1][CH:2]([O:6][CH:8]1[CH2:9][CH2:10][CH2:11][CH2:12][O:7]1)[CH2:3][C:4]#[CH:5]

参加物

5

反応物 3

HCID 80803,4-dihydro-2H-pyranHCID 929154-Pentyn-2-olHCID 161440Pyridine 4-methylbenzene-1-sulfonate

生成物 1

HCID 108990812H-Pyran, tetrahydro-2-[(1-methyl-3-butynyl)oxy]-

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

(+/−)-4-Pentyn-2-ol (5.58 ml, 59.4 mmol) and 3,4-dihydro-2H-pyran (8.08 ml, 89 mmol) were dissolved in DCM (100 ml). 4-Toluenesulfonic acid pyridine salt (1.494 g, 5.94 mmol) was added and the resulting mixture was stirred for 4 h at RT with CaCl2-tube. The mixture was concentrated. 50 ml of diethyl ether was added, extracted with brine and dried with MgSO, filtered and evaporated. The product was used in the subsequent steps without further purifications. LC-MS: [M+1]=169.23.

後処理

  1. concentrationThe mixture was concentrated
  2. addition50 ml of diethyl ether was added
  3. extractionextracted with brine
  4. dry with materialdried with MgSO
  5. filtrationfiltered
  6. customevaporated

出典と根拠

ORDレコード
ord-4d067790cf264ad5b83d868f70cd05ac
出典データセット
uspto-grants-2015_03
特許番号
US08975254B2

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