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Ethyl Acetoacetate → HCID 19967112, 화합물

HRID 976326
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HRID 976326 반응식
[N:1]1([CH2:6][C:7]2[CH:12]=[CH:11][C:10]([NH2:13])=[CH:9][CH:8]=2)[CH:5]=[CH:4][N:3]=[CH:2]1.O=[C:15]([CH3:22])[CH2:16][C:17](OCC)=[O:18].C(=O)([O-])[O-].[K+].[K+]>O>[N:1]1([CH2:6][C:7]2[CH:12]=[C:11]3[C:10](=[CH:9][CH:8]=2)[NH:13][C:15]([CH3:22])=[CH:16][C:17]3=[O:18])[CH:5]=[CH:4][N:3]=[CH:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8868Ethyl AcetoacetateHCID 11430Potassium CarbonateHCID 12653191-(4-Aminobenzyl)-1H-imidazole

생성물 1

HCID 19967112HCID 19967112, 화합물수율 14.4%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a stirred and heated (100° C.) solution of 10 parts of 4-(1H-imidazol-1-ylmethyl)benzenamine in 50 parts of poly phosphoric acid were added 15 parts of ethyl 3-oxobutanoate. The whole was stirred for 4 hours at 140° C. 100 Parts of water were added to the mixture and the whole was neutralized with potassium carbonate. The product was extracted with a mixture of ethyl acetate and methanol. The extract was dried, filtered and concentrated. The concentrate was crystallized from a mixture of 2-propanone and methanol. The product was filtered off and dried, yielding 2 parts (14.4%) of 6-(1H-imidazol-1-ylmethyl)-2-methyl-4(1H)-quinolinone; mp. 245.5° C. (decomp.) (compound 77).

후처리

  1. stirringThe whole was stirred for 4 hours at 140° C
  2. extractionThe product was extracted with a mixture of ethyl acetate and methanol
  3. customThe extract was dried
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe concentrate was crystallized from a mixture of 2-propanone and methanol
  7. filtrationThe product was filtered off
  8. customdried

출처 및 근거

ORD 기록
ord-10c5f157435d4c8a858a58c6ca0dd016
출처 데이터셋
uspto-grants-1997_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05612354

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