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

HRID 361887ノート

反応式

HRID 361887 の反応式
[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

参加物

5

反応物 2

HCID 80803,4-dihydro-2H-pyran2 回HCID 13851838Methyl 6-hydroxymethyl-5,6,7,8-tetrahydro-2-naphthalenecarboxylate

生成物 1

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

試薬・触媒・溶媒 2

HCID 1118Sulfuric Acid触媒2 回HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-91aeb008473d43ad9bef7f0b7f90ec39
出典データセット
uspto-grants-1999_02
特許番号
US05866577

反応ノート

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