Acetic Anhydride → N-Acenaphthen-5-ylacetamide

HRID 1951

반응식

HRID 1951 반응식
[NH2:1][C:2]1[C:12]2[C:13]3[C:5]([CH2:6][CH2:7][C:8]=3[CH:9]=[CH:10][CH:11]=2)=[CH:4][CH:3]=1.[C:14](OC(=O)C)(=[O:16])[CH3:15]>C(O)(=O)C>[C:14]([NH:1][C:2]1[C:12]2[C:13]3[C:5]([CH2:6][CH2:7][C:8]=3[CH:9]=[CH:10][CH:11]=2)=[CH:4][CH:3]=1)(=[O:16])[CH3:15]

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 625475-Aminoacenaphthene2회

생성물 1

HCID 343948N-Acenaphthen-5-ylacetamide수율 96.4%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
60 °C

실험 절차

50 ml of glacial acetic acid was added to 6.77 g (0.04 mol) of 5-aminoacenaphthene and the mixture was stirred at 60° C. to dissolve, and 8.16 g (0.08 mol) acetic anhydride was dropwise added thereto for 15 minutes. After finishing the dropwise addition, the mixture was stirred at the same temperature for 2 hours. The reaction was determined to be finished when disappearance of 5-aminoacenaphthene was identified. The reaction product was poured into 500 ml of ice water to precipitate a crystal, which was then filtrated, washed with water and dried. As this result, 8.15 g (yield: 96.4%, melting point: 180.0°-186.0° C.) of 5-(N-acetylamino)acenaphthene was obtained.

후처리

  1. dissolutionto dissolve
  2. additionthe dropwise addition
  3. stirringthe mixture was stirred at the same temperature for 2 hours
  4. customto precipitate a crystal, which
  5. filtrationwas then filtrated
  6. washwashed with water
  7. customdried

출처 및 근거

ORD 기록
ord-f7732a0ba48b458e9add51628a8da0ea
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05728500

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