Citric Acid → 2-Methylphenethyl alcohol

HRID 464928

反応式

HRID 464928 の反応式
[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]

参加物

5

反応物 3

HCID 311Citric Acid2 回HCID 96266IsochromaneHCID 178418361HCID 178418361、化合物

生成物 1

HCID 882672-Methylphenethyl alcohol

試薬・触媒・溶媒 1

HCID 23938Palladium触媒

反応条件

温度
150 °C

実験手順

1250 Grams of isochroman having the structure: ##STR64## 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:

後処理

  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

出典と根拠

ORDレコード
ord-3f040df172a14e45bd2416aeb5facb65
出典データセット
uspto-grants-1985_10
特許番号
US04549983

関連ノート

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