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Sulfuric Acid → HCID 19967123, 화합물

HRID 2081612
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인쇄 미리보기

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HRID 2081612 반응식
[N:1]1([CH2:6][C:7]2[CH:12]=[CH:11][C:10]([NH:13][C:14](=[O:19])[CH2:15][C:16](=O)[CH3:17])=[CH:9][CH:8]=2)[CH:5]=[CH:4][N:3]=[CH:2]1.S(=O)(=O)(O)O.[OH-].[NH4+]>>[N:1]1([CH2:6][C:7]2[CH:12]=[C:11]3[C:10](=[CH:9][CH:8]=2)[NH:13][C:14](=[O:19])[CH:15]=[C:16]3[CH3:17])[CH:5]=[CH:4][N:3]=[CH:2]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 1118Sulfuric AcidHCID 14923Ammonium HydroxideHCID 19967135HCID 19967135, 화합물

생성물 1

HCID 19967123HCID 19967123, 화합물수율 34.8%

반응 조건

온도
70 °C

실험 절차

7 Parts of N-[4-(1H-imidazol-1-ylmethyl)phenyl]-3-oxobutanamide were added dropwise to 73.6 parts of concentrated sulfuric acid (exothermic reaction, the temperature rose to 90° C.). Upon complete addition, the mixture was stirred for 1 hour at 70° C. The reaction mixture was poured into crushed ice and the whole was neutralized with an ammonium hydroxide solution to pH 9. The precipitated product was filtered off and taken up in water. The whole was extracted with dichloromethane. The aqueous layer was concentrated. The crystallized product was filtered off, washed with 2-propanone and dried in vacuo at 100° C., yielding 2.25 parts (34.8%) of 6-(1H-imidazol-1-ylmethyl)-4-methyl-2(1H)-quinolinone; mp. 266.0° C. (compound 1).

후처리

  1. customexothermic reaction
  2. customrose to 90° C.
  3. additionUpon complete addition
  4. additionThe reaction mixture was poured
  5. custominto crushed ice
  6. filtrationThe precipitated product was filtered off
  7. extractionThe whole was extracted with dichloromethane
  8. concentrationThe aqueous layer was concentrated
  9. filtrationThe crystallized product was filtered off
  10. washwashed with 2-propanone
  11. customdried in vacuo at 100° C.

출처 및 근거

ORD 기록
ord-5575c2b540234ba7a39bbe867a74b0ec
출처 데이터셋
uspto-grants-1993_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05185346

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