Methyl 2-hydroxy-1-naphthoate → Methyl 2-hydroxy-5,6,7,8-tetrahydronaphthalene-1-carboxylate

HRID 259010

反応式

HRID 259010 の反応式
[OH:1][C:2]1[CH:11]=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]=1[C:12]([O:14][CH3:15])=[O:13].[H][H]>[Pd].C(O)(=O)C>[OH:1][C:2]1[CH:11]=[CH:10][C:9]2[CH2:8][CH2:7][CH2:6][CH2:5][C:4]=2[C:3]=1[C:12]([O:14][CH3:15])=[O:13]

参加物

5

反応物 2

HCID 598533Methyl 2-hydroxy-1-naphthoateHCID 178418361HCID 178418361、化合物2 回

生成物 1

HCID 11600901Methyl 2-hydroxy-5,6,7,8-tetrahydronaphthalene-1-carboxylate

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 176Acetic Acid溶媒

実験手順

In 2.5 l. of glacial acetic acid is dissolved 417 g. of methyl 2-hydroxy-1-naphthoate, and with the addition of 150 g. of 5% palladium-on-carbon, reduction is carried out at a temperature of 60° to 80° C with hydrogen introduced at a pressure of 100kg./cm2. In 3 hours, approximately 2 moles of hydrogen is absorbed. The reaction mixture is filtered and the filtrate is concentrated under reduced pressure. The residue is then subjected to distillation under reduced pressure and the fraction boiling at 123° -125° C (0.6 mmHg) is recovered to obtain methyl 2-hydroxy-5,6,7,8-tetrahydro-1-naphthoate as a colorless oil. The oil solidifies on standing in the cold.

後処理

  1. additionintroduced at a pressure of 100kg
  2. filtrationThe reaction mixture is filtered
  3. concentrationthe filtrate is concentrated under reduced pressure
  4. distillationThe residue is then subjected to distillation under reduced pressure
  5. customthe fraction boiling at 123° -125° C (0.6 mmHg) is recovered

出典と根拠

ORDレコード
ord-2126f8ab992c4dcc9337b56ee47aa1d9
出典データセット
uspto-grants-1977_07
特許番号
US04035512

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