Water → 7-Methoxy-4-methyl-2H-1-benzopyran

HRID 236979노트

반응식

HRID 236979 반응식
O[C:2]1([CH3:14])[C:7]2[CH:8]=[CH:9][C:10]([O:12][CH3:13])=[CH:11][C:6]=2[O:5][CH2:4][CH2:3]1.P(Cl)(Cl)(Cl)=O.O>N1C=CC=CC=1>[CH3:13][O:12][C:10]1[CH:9]=[CH:8][C:7]2[C:2]([CH3:14])=[CH:3][CH2:4][O:5][C:6]=2[CH:11]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 24813Phosphorus oxychlorideHCID 203045882,3-Dihydro-4-hydroxy-7-methoxy-4-methyl-4H-1-benzopyran

생성물 1

HCID 122094127-Methoxy-4-methyl-2H-1-benzopyran

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

The carbinol of step (a) (73.3 g) was stirred with phosphorus oxychloride (19.3 g; 11.6 ml) in dry pyridine (380 ml) for 20 hours under nitrogen. The reaction mixture was poured into water, extracted with ether and the ethereal extracts were washed with dilute acid, then sodium bicarbonate solution, then water and dried. Evaporation of the solvent left 58 g of residue (87.2%). MS evidence was correct for the required compound. NMR suggested that the product was in fact a mixture of isomeric alkenes.

후처리

  1. extractionextracted with ether
  2. washthe ethereal extracts were washed
  3. additionwith dilute acid
  4. dry with materialsodium bicarbonate solution, then water and dried
  5. customEvaporation of the solvent
  6. waitleft 58 g of residue (87.2%)
  7. additiona mixture of isomeric alkenes

출처 및 근거

ORD 기록
ord-9c2f445cdf7743dcb734cdd9167845de
출처 데이터셋
uspto-grants-1979_06
특허 번호
US04159273

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