Citric Acid → 2-Methylphenethyl alcohol

HRID 364335

반응식

HRID 364335 반응식
[CH2:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3][O:2]1.C(O)(=O)CC(CC(O)=O)(C(O)=O)O.[H][H]>[Pd]>[CH3:1][C:10]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[CH2:4][CH2:3][OH:2]

참가 물질

5

반응물 3

HCID 311Citric Acid2회HCID 96266IsochromaneHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 882672-Methylphenethyl alcohol

시약·촉매·용매 1

HCID 23938Palladium촉매

반응 조건

온도
150 °C

실험 절차

1250 Grams of isochroman having the structure: ##STR63## 25 grams of 5% palladium-on-carbon and 12.5 grams of citric acid are placed in a 4-liter autoclave. The autoclave is sealed, heated to 150° C. and pressurized with hydrogen at 200 psig. After five hours, 12.5 grams of additional citric acid is added to the autoclave and the autoclave is resealed. The autoclave is then heated at a pressure of 200 psig and 150° C. for an additional three hours. At the end of this additional three hour period, the autoclave is opened, the contents filtered and the filtrate is distilled over 2 grams of calcium carbonate through a 24" Goodloe column yielding the following fractions:

후처리

  1. customThe autoclave is sealed
  2. temperatureThe autoclave is then heated at a pressure of 200 psig and 150° C. for an additional three hours
  3. customAt the end of this additional three hour period
  4. filtrationthe contents filtered
  5. distillationthe filtrate is distilled over 2 grams of calcium carbonate through a 24" Goodloe column
  6. customyielding the following fractions

출처 및 근거

ORD 기록
ord-d34391ea0bf845ffb38507f255ff0f8e
출처 데이터셋
uspto-grants-1986_08
특허 번호
US04604487

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