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

HRID 872884

반응식

HRID 872884 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

(+/−)-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.

후처리

  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

출처 및 근거

ORD 기록
ord-4d067790cf264ad5b83d868f70cd05ac
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08975254B2

연결된 노트

불러오는 중…