2-Nitropropane → HCID 14478920、化合物

HRID 620005ノート

反応式

HRID 620005 の反応式
C[O-].[Na+].[N+](C(C)C)([O-])=[O:5].[CH3:10][C:11]1[C:18]([CH2:19]Br)=[CH:17][CH:16]=[C:15]([NH:21][C:22](=[O:24])[CH3:23])[C:12]=1[C:13]#[N:14]>CO>[C:22]([NH:21][C:15]1[CH:16]=[CH:17][C:18]([CH:19]=[O:5])=[C:11]([CH3:10])[C:12]=1[C:13]#[N:14])(=[O:24])[CH3:23]

参加物

5

反応物 3

HCID 3982-NitropropaneHCID 10942334Sodium MethoxideHCID 14478919HCID 14478919、化合物

生成物 1

HCID 14478920HCID 14478920、化合物収率 53%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of sodium methoxide, 0.43 g, in 100 ml of methanol, was added 0.84 g of 2-nitropropane. After 15 min, 2 g of 2-methyl-3-bromomethyl-6-acetamidobenzonitrile was added and the resulting solution was stirred for 2.5 h at ambient temperature. The solvent was then evaporated at reduced pressure and the residue dissolved in chloroform. The chloroform solution was filtered, washed with H2O, dried and the solvent removed at reduced pressure. The residue was crystallized from chloroform-carbon tetrachloride to yield 0.8 g (53%) of product, m.p. 170°-173° C. NMR (CDCl3) 2.30 (3H, s, CH3CO--N), 2.90 (3H, s, CH3), 8.00 (1H, d, C--5H), 8.6 (1H, d, C--6H), 10.20 (1H, s, (CHO)d. Anal. calc'd for CH11H10N2O2.1/3H2O: C, 63.5; H, 4.84; N, 13.5. Found: C, 63.4; H, 5.00; N, 13.7.

後処理

  1. customThe solvent was then evaporated at reduced pressure
  2. dissolutionthe residue dissolved in chloroform
  3. filtrationThe chloroform solution was filtered
  4. washwashed with H2O
  5. customdried
  6. customthe solvent removed at reduced pressure
  7. customThe residue was crystallized from chloroform-carbon tetrachloride

出典と根拠

ORDレコード
ord-7119c987ffdf4914bbf95d3170801949
出典データセット
uspto-grants-1989_04
特許番号
US04818753

反応ノート

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