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

HRID 259010

반응식

HRID 259010 반응식
[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]

참가 물질

5

반응물 2

HCID 598533Methyl 2-hydroxy-1-naphthoateHCID 178418361HCID 178418361, 화합물2회

생성물 1

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

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2126f8ab992c4dcc9337b56ee47aa1d9
출처 데이터셋
uspto-grants-1977_07
특허 번호
US04035512

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