Water → Florfenicol phthalate

HRID 1444590노트

반응식

HRID 1444590 반응식
[CH3:1][S:2]([C:5]1[CH:6]=[CH:7][C:8]([C@@H:11]([OH:21])[C@H:12]([NH:15][C:16]([CH:18]([Cl:20])[Cl:19])=[O:17])[CH2:13][F:14])=[CH:9][CH:10]=1)(=[O:4])=[O:3].[C:22]1(=[O:32])[O:27][C:25](=[O:26])[C:24]2=[CH:28][CH:29]=[CH:30][CH:31]=[C:23]12.C(N(CC)CC)C.[OH2:40]>O1CCOCC1.ClCCl>[CH3:1][S:2]([C:5]1[CH:6]=[CH:7][C:8]([C@@H:11]([OH:21])[C@H:12]([NH:15][C:16]([CH:18]([Cl:20])[Cl:19])=[O:17])[CH2:13][F:14])=[CH:9][CH:10]=1)(=[O:4])=[O:3].[C:25]([O-:27])(=[O:26])[C:24]1[C:23](=[CH:31][CH:30]=[CH:29][CH:28]=1)[C:22]([O-:32])=[O:40]

참가 물질

7

반응물 4

HCID 962WaterHCID 6811Phthalic AnhydrideHCID 8471TriethylamineHCID 114811Florfenicol

생성물 1

HCID 86596089Florfenicol phthalate

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 312751,4-Dioxane용매

실험 절차

3.9 g of florfenicol, 3.6 g of phthalic anhydride and 7.2 ml of triethyl amine in 36 ml of dioxane were taken in a 100 ml round bottom flask equipped with a magnetic stir bar and a drying tube. The reaction mixture was stirred at room temperature for 6 hours. After 6 hours, the contents were poured into 300 ml of cold water. The resulting gummy solid was dissolved in dichloromethane and washed thoroughly with saturated bicarbonate several times followed by water. The organic layer was dried over anhydrous sodium sulfate and concentrated over roto-evaporator. The semisolid obtained was recrystallized in a mixture of ethylacetate and hexane to obtain a solid product of 4.2 grams.

후처리

  1. customequipped with a magnetic stir bar and a drying tube
  2. waitAfter 6 hours
  3. washwashed thoroughly with saturated bicarbonate several times
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. concentrationconcentrated over roto-evaporator
  6. customThe semisolid obtained
  7. customwas recrystallized in a mixture of ethylacetate and hexane
  8. customto obtain a solid product of 4.2 grams

출처 및 근거

ORD 기록
ord-d7e8a04f1add4119ad0137e311102ae7
출처 데이터셋
uspto-grants-2010_02
특허 번호
US07662861B2

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