Sodium Carbonate → 1,3-Dichloroisoquinoline

HRID 1006876

反応式

HRID 1006876 の反応式
[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

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 3494351,3(2H,4H)-isoquinolinedioneHCID 22048082HCID 22048082、化合物

生成物 1

HCID 2986251,3-Dichloroisoquinoline

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-6979a33c740f4041a597c027f56fc455
出典データセット
uspto-grants-2004_09
特許番号
US06790844B2

関連ノート

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