Nitrogen → Methyl (5-fluoro-2-methyl-1H-inden-3-yl)acetate

HRID 567192노트

반응식

HRID 567192 반응식
N(CN[C:5](N)=[O:6])=O.[OH-].[K+].[F:10][C:11]1[CH:12]=[C:13]2[C:17](=[CH:18][CH:19]=1)[CH2:16][C:15]([CH3:20])=[C:14]2[CH2:21][C:22](O)=[O:23].N#N>ClCCl.C(OCC)C>[F:10][C:11]1[CH:12]=[C:13]2[C:17](=[CH:18][CH:19]=1)[CH2:16][C:15]([CH3:20])=[C:14]2[CH2:21][C:22]([O:6][CH3:5])=[O:23]

참가 물질

7

반응물 4

HCID 947NitrogenHCID 14797Potassium HydroxideHCID 104823Urea, (nitrosomethyl)-HCID 30156085-Fluoro-2-methyl-1H-indene-3-acetic acid

생성물 1

HCID 15434585Methyl (5-fluoro-2-methyl-1H-inden-3-yl)acetate수율 93%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6344Dichloromethane용매

실험 절차

Nitrosomethylurea (99.5 mmol) is added in portions to a cold (0° C.) mixture of aqueous 50% KOH (50 ml) and diethylether (150 ml) at 0° C. The yellow ether solution of diazomethane (Note: explosive) is separated, is washed with water, and is added in portions to a solution of 5-fluoro-2-methylindene-3-acetic acid (90 mmol) in dichloromethane (200 ml). When the evolution of N2 ceases, the reaction is complete. After evaporation of the solvents, the residue is recrystallized from hexane to give methyl 5-fluoro-2-methyl-3-indenylacetate (yield 93%; m.p. 53° C.).

후처리

  1. customThe yellow ether solution of diazomethane (Note: explosive) is separated
  2. washis washed with water
  3. customAfter evaporation of the solvents
  4. customthe residue is recrystallized from hexane

출처 및 근거

ORD 기록
ord-640f6b0c2e5e4c86baabf1baee723f27
출처 데이터셋
uspto-grants-2001_01
특허 번호
US06177471B1

반응 노트

불러오는 중…