Sodium Carbonate → 1,3-Dichloroisoquinoline

HRID 1006876

반응식

HRID 1006876 반응식
[C:1]1(=O)[NH:6][C:5](=O)[C:4]2=[CH:8][CH:9]=[CH:10][CH:11]=[C:3]2[CH2:2]1.[Cl-:13].[Cl-:14].C1(P(=O)([O-])[O-])C=CC=CC=1.C(=O)([O-])[O-].[Na+].[Na+]>O>[Cl:13][C:5]1[C:4]2[C:3](=[CH:11][CH:10]=[CH:9][CH:8]=2)[CH:2]=[C:1]([Cl:14])[N:6]=1

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 3494351,3(2H,4H)-isoquinolinedioneHCID 22048082HCID 22048082, 화합물

생성물 1

HCID 2986251,3-Dichloroisoquinoline

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture solution of homophthalimide (10.5 g) and phenylphosphonate dichloride (30 ml) was heated at 110° C. for 2 hr. After the reaction mixture was cooled, water was added thereto, and then the resulting mixture was neutralized with sodium carbonate. The resulting mixture was extracted with ethyl acetate, washed with brine, dried, and then the solvent was evaporated. The resulting residue was purified by silica gel column chromatography (methylene chloride), to give 9.30 g of the title compound as white crystals.

후처리

  1. temperatureAfter the reaction mixture was cooled
  2. extractionThe resulting mixture was extracted with ethyl acetate
  3. washwashed with brine
  4. customdried
  5. customthe solvent was evaporated
  6. customThe resulting residue was purified by silica gel column chromatography (methylene chloride)

출처 및 근거

ORD 기록
ord-6979a33c740f4041a597c027f56fc455
출처 데이터셋
uspto-grants-2004_09
특허 번호
US06790844B2

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