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2-Amino-2,3-dimethylbutanamide → HCID 67643449、化合物

HRID 1974465
ノート
印刷プレビュー

反応式

HRID 1974465 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 97937732-Amino-2,3-dimethylbutanamideHCID 15672406HCID 15672406、化合物HCID 23665647Potassium tert-butoxide

生成物 1

HCID 67643449HCID 67643449、化合物収率 213.5%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a stirred solution of dimethyl 5-(1-acetyl-3-methyl-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 vacumn, 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.

後処理

  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 vacumn
  4. customthe product triturated with 33% ethanol in chloroform
  5. filtrationfiltered
  6. concentrationThe filtrate is concentrated in vacuo

出典と根拠

ORDレコード
ord-7b4ff25069ed4abf8edb7568f908d5ef
出典データセット
uspto-grants-1994_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05283230

反応ノート

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