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

HRID 2072317

반응식

HRID 2072317 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-cd0a699458314b2ba21c7bbbcea18164
출처 데이터셋
uspto-grants-1977_09
특허 번호
US04051152

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