Acetic Anhydride → 5-Acetamido-phthalide

HRID 322231

반응식

HRID 322231 반응식
[NH2:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[C:7](=[O:8])[O:6][CH2:5]2.C(N(CC)CC)C.[C:19](OC(=O)C)(=[O:21])[CH3:20].C(=O)([O-])O.[Na+]>O1CCCC1>[C:19]([NH:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[C:7](=[O:8])[O:6][CH2:5]2)(=[O:21])[CH3:20]

참가 물질

6

반응물 4

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 516892Sodium BicarbonateHCID 7206695-Aminophthalide

생성물 1

HCID 5909685-Acetamido-phthalide수율 97.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

In tetrahydrofuran (100 ml) was dissolved 5-aminophthalide (10 g, 67.05 mmol), and triethylamine (18.64 ml, 134 mmol) was added thereto. To the resulting mixture was added dropwise acetic anhydride (12.61 ml, 134 mmol) under ice-cooling, followed by stirring at room temperature for 3 hours. After addition of a 5% aqueous solution of sodium hydrogen carbonate, the precipitated white solid was separated by filtration, washed several times with water, and then dried to give 5-acetamidophthalide (12.45 g, 97%).

후처리

  1. additionwas added
  2. temperaturecooling
  3. customthe precipitated white solid was separated by filtration
  4. washwashed several times with water
  5. customdried

출처 및 근거

ORD 기록
ord-4e7e08e7ad624f8b9f0d0f3875001415
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06211227B1

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