Methylamine → HCID 83702359、化合物

HRID 1055661ノート

反応式

HRID 1055661 の反応式
[C:1]([C:5]1[CH:6]=[C:7]([CH:12]=[C:13](Cl)[N:14]=1)[C:8]([O:10]C)=[O:9])([CH3:4])([CH3:3])[CH3:2].[CH3:16][NH2:17]>>[C:1]([C:5]1[CH:6]=[C:7]([CH:12]=[C:13]([NH:17][CH3:16])[N:14]=1)[C:8]([OH:10])=[O:9])([CH3:4])([CH3:3])[CH3:2]

参加物

3

反応物 2

HCID 6329MethylamineHCID 86690963Methyl 2-chloro-6-(1,1-dimethylethyl)-4-pyridinecarboxylate

生成物 1

HCID 83702359HCID 83702359、化合物

反応条件

温度
130 °C

実験手順

1.0 g (4.39 mmol) of methyl 2-tert-butyl-6-chloroisonicotinate [lit.: O. Isler et al., Helvetica Chimica Acta 1955, 38 (4), 1033-1046] and 3.8 ml (43.9 mmol) of a 40% strength aqueous methylamine solution were heated in a microwave oven (Biotage Initiator, with Dynamic Field Tuning) at 160° C. for 6 h. After cooling, the volatile components were removed on a rotary evaporator. The residue was taken up in 4 ml of semiconcentrated hydrochloric acid and once more heated in the microwave at 130° C. for 1 h. The product was then isolated directly by preparative HPLC (Method 12). Evaporation of the product fractions and drying of the residue under high vacuum gave 180 mg (92% pure, 18% of theory) of the title compound.

後処理

  1. temperatureAfter cooling
  2. customthe volatile components were removed on a rotary evaporator
  3. customThe product was then isolated directly by preparative HPLC (Method 12)
  4. customEvaporation of the product fractions
  5. customdrying of the residue under high vacuum

出典と根拠

ORDレコード
ord-82cd0cbe09a344a2bab0fa75633040ca
出典データセット
uspto-grants-2016_07
特許番号
US09394309B2

反応ノート

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