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2-Amino-2,3-dimethylbutanamide → HCID 67643449, 화합물

HRID 2255215
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HRID 2255215 반응식
[C:1]([N:4]1[CH2:8][CH2:7][N:6]([CH3:9])[CH:5]1[C:10]1[CH:11]=[C:12]([C:20]([O:22]C)=[O:21])[C:13]([C:16](OC)=O)=[N:14][CH:15]=1)(=[O:3])[CH3:2].[NH2:24][C:25]([CH3:32])([CH:29]([CH3:31])[CH3:30])[C:26]([NH2:28])=[O:27].CC(C)([O-])C.[K+]>C1(C)C=CC=CC=1>[NH4+:4].[C:1]([N:4]1[CH2:8][CH2:7][N:6]([CH3:9])[CH:5]1[C:10]1[CH:15]=[N:14][C:13]([C:16]2[NH:28][C:26](=[O:27])[C:25]([CH:29]([CH3:31])[CH3:30])([CH3:32])[N:24]=2)=[C:12]([CH:11]=1)[C:20]([O-:22])=[O:21])(=[O:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 97937732-Amino-2,3-dimethylbutanamideHCID 15672406HCID 15672406, 화합물HCID 23665647Potassium tert-butoxide

생성물 1

HCID 67643449HCID 67643449, 화합물수율 213.5%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To a stirred solution of dimethyl 5-(1-acetyl-3methyl-2-imidazolidinyl)pyridine-2,3-dicarboxylate (0.70 g, 0.0022 mol), and 2-amino-2,3-dimethylbutyramide (0.28 g, 0.0022 mol) in toluene (10 mL) is added potassium tert-butoxide (0.49 g, 0.0044 mol). The resulting mixture is stirred for 2 hours at 80° C. to 90° C. After cooling to room temperature, the reaction is quenched by the addition of water (15 mL) and ammonium chloride (0.25 g). The layers are separated, the aqueous solution concentrated under high vacuum, the product triturated with 33% ethanol in chloroform and filtered. The filtrate is concentrated in vacuo to afford the title compound (0.95 g, 100%) as a gold solid, mp 93°-98° C., identified by IR and NMR spectral analyses.

후처리

  1. customthe reaction is quenched by the addition of water (15 mL) and ammonium chloride (0.25 g)
  2. customThe layers are separated
  3. concentrationthe aqueous solution concentrated under high vacuum
  4. customthe product triturated with 33% ethanol in chloroform
  5. filtrationfiltered
  6. concentrationThe filtrate is concentrated in vacuo

출처 및 근거

ORD 기록
ord-811e57a7a6ed423aa2509eef79721069
출처 데이터셋
uspto-grants-1993_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05239070

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