Ethyl Acetate → HCID 53883802, 화합물

HRID 365347노트

반응식

HRID 365347 반응식
[CH:1]([O:4][C:5]([C:7]1[N:8]=[CH:9][C:10]2[NH:11][C:12]3[C:17]([C:18]=2[C:19]=1[CH2:20][CH3:21])=[CH:16][C:15]([NH:22][C:23](=O)[CH3:24])=[CH:14][CH:13]=3)=[O:6])([CH3:3])[CH3:2].COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:35])=CC=1.C(OCC)(=O)C>O1CCOCC1>[CH:1]([O:4][C:5]([C:7]1[N:8]=[CH:9][C:10]2[NH:11][C:12]3[C:17]([C:18]=2[C:19]=1[CH2:20][CH3:21])=[CH:16][C:15]([NH:22][C:23](=[S:35])[CH3:24])=[CH:14][CH:13]=3)=[O:6])([CH3:3])[CH3:2]

참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 87949Lawesson's reagentHCID 54114684HCID 54114684, 화합물

생성물 1

HCID 53883802HCID 53883802, 화합물수율 53.7%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

2741 mg of 6-acetylamino-4-ethyl-β-carboline-3-carboxylic acid isopropyl ester is heated to 70° C. in 110 ml of dioxane with 3915 mg of Lawesson's reagent while being stirred. After cooling, it is mixed with 100 ml of ethyl acetate and washed with saturated sodium chloride solution. The organic phases are dried and concentrated by evaporation in a vacuum. The residue is chromatographed on silica gel with toluene+methanol=8+2. 1541 mg of 4-ethyl-6-thioacetylamino-β-carboline-3-carboxylic acid isopropyl ester with a melting point of 158-160° C. is obtained from the desired fractions.

후처리

  1. temperatureAfter cooling
  2. washwashed with saturated sodium chloride solution
  3. customThe organic phases are dried
  4. concentrationconcentrated by evaporation in a vacuum
  5. customThe residue is chromatographed on silica gel with toluene+methanol=8+2

출처 및 근거

ORD 기록
ord-13b3ea3ebcb8487696dff6f1cce816f1
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06127368

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