3,4-dihydro-2H-pyran → Methyl 6-[(2-tetrahydropyranyl)oxymethyl]-5,6,7,8-tetrahydro-2-naphthalenecarboxylate

HRID 1901317노트

반응식

HRID 1901317 반응식
[OH:1][CH2:2][CH:3]1[CH2:12][CH2:11][C:10]2[CH:9]=[C:8]([C:13]([O:15][CH3:16])=[O:14])[CH:7]=[CH:6][C:5]=2[CH2:4]1.[O:17]1[CH:22]=[CH:21][CH2:20][CH2:19][CH2:18]1>S(=O)(=O)(O)O.C(OCC)C>[O:17]1[CH2:22][CH2:21][CH2:20][CH2:19][CH:18]1[O:1][CH2:2][CH:3]1[CH2:12][CH2:11][C:10]2[CH:9]=[C:8]([C:13]([O:15][CH3:16])=[O:14])[CH:7]=[CH:6][C:5]=2[CH2:4]1

참가 물질

5

반응물 2

HCID 80803,4-dihydro-2H-pyran2회HCID 13851838Methyl 6-hydroxymethyl-5,6,7,8-tetrahydro-2-naphthalenecarboxylate

생성물 1

HCID 21844324Methyl 6-[(2-tetrahydropyranyl)oxymethyl]-5,6,7,8-tetrahydro-2-naphthalenecarboxylate수율 99.3%

시약·촉매·용매 2

HCID 1118Sulfuric Acid촉매2회HCID 3283Diethyl Ether용매

실험 절차

10.0 g of methyl 6-hydroxymethyl-5,6,7,8-tetrahydro-2-naphthalenecarboxylate was added to 3.82 g of 2,3-dihydropyrane. After further adding 5 drops of concentrated sulfuric acid, the resulting mixture was stirred for 1 hour. To this were further added 1.00 g of 2,3-dihydropyrane and 3 drops of concentrated sulfuric acid, followed by stirring for 5 hours. The resulting reaction mixture was mixed with 100 ml of diethyl ether, and the mixture was washed with saturated sodium bicarbonate aqueous solution, water and saturated sodium chloride aqueous solution in that order, followed by drying. By distilling off the solvent, 13.72 g of methyl 6-[(2-tetrahydropyranyl)oxymethyl]-5,6,7,8-tetrahydro-2-naphthalenecarboxylate was obtained in the form of yellow oil.

후처리

  1. stirringby stirring for 5 hours
  2. customThe resulting reaction mixture
  3. washthe mixture was washed with saturated sodium bicarbonate aqueous solution, water and saturated sodium chloride aqueous solution in that order
  4. customby drying
  5. distillationBy distilling off the solvent

출처 및 근거

ORD 기록
ord-9886009ca187403bb79a0f5ed9b20010
출처 데이터셋
uspto-grants-1996_11
특허 번호
US05576343

반응 노트

불러오는 중…