Acetic Anhydride → 1-Acetyl-1H-indol-3-yl acetate

HRID 1162165

반응식

HRID 1162165 반응식
[C:1]([O:4][C:5](=O)[CH3:6])(=[O:3])[CH3:2].C(N(CC)CC)C.[C:15]([N:18]([CH2:28]C(O)=O)[C:19]1C=[CH:26][CH:25]=[CH:24][C:20]=1C(O)=O)(=[O:17])[CH3:16]>O>[C:15]([N:18]1[C:19]2[C:6](=[CH:26][CH:25]=[CH:24][CH:20]=2)[C:5]([O:4][C:1](=[O:3])[CH3:2])=[CH:28]1)(=[O:17])[CH3:16]

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 7151462-[Acetyl(carboxymethyl)amino]benzoic acid

생성물 1

HCID 5836021-Acetyl-1H-indol-3-yl acetate수율 86.3%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a stirred mixture of acetic anhydride (46.29 g, 0.45 mol) and triethylamine (13.77 g, 0.14 mol), 2-(N-acetylcarboxymethylamino)benzoic acid of Example 1b (11.36 g, 0.048 mol) was added at room temperature. The mixture was refluxed for 20 min and concentrated in vacuum to give an oily residue. Water (350 mL) was added under vigorous stirring, and the mixture was refrigerated overnight. The solid product was collected, washed with water and air-dried to give 9.0 g (86%) of the product which was used in the next step without purification.

후처리

  1. additionwas added at room temperature
  2. temperatureThe mixture was refluxed for 20 min
  3. concentrationconcentrated in vacuum
  4. customto give an oily residue
  5. customThe solid product was collected
  6. washwashed with water
  7. customair-dried

출처 및 근거

ORD 기록
ord-be5e60906ebe4785b1746ab10e2ebf17
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07820691B2

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