Acetic Anhydride → 9-Acetoxy-4,4-dimethyl-7-(1,2-dimethylheptyl)-1,2,3,4-tetrahydrocyclopenta[c][l] benzopyran

HRID 2072317ノート

反応式

HRID 2072317 の反応式
[CH3:1][C:2]1([CH3:25])[C:7]2[CH2:8][CH2:9][CH2:10][C:6]=2[C:5]2[C:11]([OH:24])=[CH:12][C:13]([CH:15]([CH3:23])[CH:16]([CH3:22])[CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])=[CH:14][C:4]=2[O:3]1.[C:26](OC(=O)C)(=[O:28])[CH3:27]>N1C=CC=CC=1>[C:26]([O:24][C:11]1[C:5]2[C:6]3[CH2:10][CH2:9][CH2:8][C:7]=3[C:2]([CH3:1])([CH3:25])[O:3][C:4]=2[CH:14]=[C:13]([CH:15]([CH3:23])[CH:16]([CH3:22])[CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])[CH:12]=1)(=[O:28])[CH3:27]

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 215348Cyclopenta(c)(1)benzopyran-9-ol, 1,2,3,4-tetrahydro-4,4-dimethyl-7-(1,2-dimethylheptyl)-

生成物 1

HCID 218539109-Acetoxy-4,4-dimethyl-7-(1,2-dimethylheptyl)-1,2,3,4-tetrahydrocyclopenta[c][l] benzopyran

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A solution of 4,4-dimethyl-9-hydroxy-7-(1,2-dimethylheptyl)-1,2,3,4-tetrahydrocyclopenta[ c][l]benzopyran (6.85 g., 0.02 mole) and acetic anhydride (3.06 g., 0.03 mole) in 20 ml. of pyridine was warmed over a steam bath with stirring for 2 hours. The reaction mixture was allowed to cool to room temperature and the pyridine was removed by evaporation under reduced pressure. Water was added to the residue and this aqueous mixture was extracted with three portions of ether. The ether extracts were washed several times with water, 6N HCl, again with water, and dried over Na2SO4. Solvent evaporation in vacuo left 7.59 g. (99%) of crude acetate. The ir and nmr were in agreement with the proposed structure.

後処理

  1. customthe pyridine was removed by evaporation under reduced pressure
  2. additionWater was added to the residue
  3. extractionthis aqueous mixture was extracted with three portions of ether
  4. washThe ether extracts were washed several times with water, 6N HCl
  5. dry with materialagain with water, and dried over Na2SO4
  6. customSolvent evaporation in vacuo
  7. waitleft 7.59 g

出典と根拠

ORDレコード
ord-cd0a699458314b2ba21c7bbbcea18164
出典データセット
uspto-grants-1977_09
特許番号
US04051152

反応ノート

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