Acetic Anhydride → 5-Acetamido-phthalide

HRID 322231

反応式

HRID 322231 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 5909685-Acetamido-phthalide収率 97.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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%).

後処理

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

出典と根拠

ORDレコード
ord-4e7e08e7ad624f8b9f0d0f3875001415
出典データセット
uspto-grants-2001_04
特許番号
US06211227B1

関連ノート

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