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7-Methoxy-3,4-dihydro-2H-1-benzopyran-3-amine--hydrogen chloride (1/1) → HCID 22100485, 화합물

HRID 1457748
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HRID 1457748 반응식
Cl.[NH2:2][CH:3]1[CH2:12][C:11]2[C:6](=[CH:7][C:8]([O:13][CH3:14])=[CH:9][CH:10]=2)[O:5][CH2:4]1.[CH3:15][O:16][C:17]1[CH:25]=[CH:24][C:23]([Cl:26])=[CH:22][C:18]=1[C:19](Cl)=[O:20]>N1C=CC=CC=1>[Cl:26][C:23]1[CH:24]=[CH:25][C:17]([O:16][CH3:15])=[C:18]([CH:22]=1)[C:19]([NH:2][CH:3]1[CH2:12][C:11]2[C:6](=[CH:7][C:8]([O:13][CH3:14])=[CH:9][CH:10]=2)[O:5][CH2:4]1)=[O:20]
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참가 물질

4

반응물 2

HCID 30416007-Methoxy-3,4-dihydro-2H-1-benzopyran-3-amine--hydrogen chloride (1/1)HCID 123841765-Chloro-2-methoxybenzoyl chloride

생성물 1

HCID 22100485HCID 22100485, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
60 °C

실험 절차

15.1 g (70 mmol) of 3-amino-7-methoxychroman hydrochloride (Eur. J. Med. Chem. 11 (1976), 251-256) were dissolved in 80 ml of pyridine, and 14.8 g of 2-methoxy-5-chlorobenzoyl chloride were added at 0° C. The mixture was stirred at room temperature for 1.5 hours and at 60° C. for 1 hour. The cooled reaction mixture was partitioned between water and methylene chloride. The aqueous phase was extracted three times with methylene chloride. The combined organic phases were washed with 2N hydrochloric acid, water and bicarbonate solution. After drying and evaporation of the organic phase, the residue was dissolved in a little toluene and the product was precipitated with excess diethyl ether. 3-(5-chloro-2-methoxybenzamido)-7-methoxychroman of melting point 92°-93° C. was obtained.

후처리

  1. customThe cooled reaction mixture
  2. customwas partitioned between water and methylene chloride
  3. extractionThe aqueous phase was extracted three times with methylene chloride
  4. washThe combined organic phases were washed with 2N hydrochloric acid, water and bicarbonate solution
  5. customAfter drying
  6. customevaporation of the organic phase
  7. dissolutionthe residue was dissolved in a little toluene
  8. customthe product was precipitated with excess diethyl ether

출처 및 근거

ORD 기록
ord-d8e777ce2dad42efa9b7462aa268c901
출처 데이터셋
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05849755

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