Triethylamine → HCID 22715001、化合物

HRID 352013ノート

反応式

HRID 352013 の反応式
[Cl:1][C:2]1[C:7]([NH2:8])=[C:6]([NH:9][CH2:10][CH:11]([CH3:13])[CH3:12])[CH:5]=[C:4]([CH3:14])[N:3]=1.C(N(CC)CC)C.[CH2:22]([O:24][CH2:25][C:26](Cl)=[O:27])[CH3:23]>ClCCl>[Cl:1][C:2]1[C:7]([NH:8][C:26](=[O:27])[CH2:25][O:24][CH2:22][CH3:23])=[C:6]([NH:9][CH2:10][CH:11]([CH3:12])[CH3:13])[CH:5]=[C:4]([CH3:14])[N:3]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 84189Ethoxyacetyl chlorideHCID 227150032-Chloro-N4-(2-methylpropyl)-6-methylpyridin-3,4-diamine

生成物 1

HCID 22715001HCID 22715001、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

Anhydrous dichloromethane (750 ml) and 2-chloro-N4-(2-methylpropyl)-6-methylpyridin-3,4-diamine (18.84 g) were combined and cooled to 0° C. Triethylamine (12.9 ml) was added dropwise to the resulting mixture, and then ethoxyacetyl chloride (11.34 g) dissolved in anhydrous dichloromethane (50 ml) was added slowly to the resulting mixture, which turned dark. After two hours the dark mixture was allowed to warm to room temperature. TLC analysis of the reaction mixture indicated completion, and the solvent was removed under reduced pressure. The resulting yellow solid was dissolved in chloroform, and the resulting solution was washed with water. The organic layer was dried with magnesium sulfate and concentrated to a dark brown oil (27.75 g) under reduced pressure. NMR analysis of the oil indicated desired product of suitable purity for use in the next step.

後処理

  1. additionwas added slowly to the resulting mixture, which
  2. temperatureto warm to room temperature
  3. customthe solvent was removed under reduced pressure
  4. dissolutionThe resulting yellow solid was dissolved in chloroform
  5. washthe resulting solution was washed with water
  6. dry with materialThe organic layer was dried with magnesium sulfate
  7. concentrationconcentrated to a dark brown oil (27.75 g) under reduced pressure

出典と根拠

ORDレコード
ord-ca1589a51e0d4996bf9068ed833c9673
出典データセット
uspto-grants-2004_06
特許番号
US06743920B2

反応ノート

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