1,2-Dimethoxyethane → Pyridine-2,3-dicarboxamide

HRID 330363ノート

反応式

HRID 330363 の反応式
[NH2:1][CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N:4]=1.ClC[C:11]([N:13](CCCC)CCCC)=[O:12].C(N(C(C)C)CC)(C)C.C(COC)[O:32]C>C(Cl)Cl>[N:4]1[CH:5]=[CH:6][CH:7]=[C:8]([C:11]([NH2:13])=[O:12])[C:3]=1[C:2]([NH2:1])=[O:32]

参加物

6

反応物 4

HCID 80711,2-DimethoxyethaneHCID 195092-PyridinemethanamineHCID 81531DiisopropylethylamineHCID 222374N,N-Dibutyl-2-chloroacetamide

生成物 1

HCID 578921Pyridine-2,3-dicarboxamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Pyridine diamide 6 was prepared according to the general procedure described in Example 8 using 2-(aminomethyl)pyridine (0.010 mol), 2-chloro-N,N-dibutylacetamide (0.030 mol), diisopropylethylamine (0.030 mol) and dimethoxyethane (30 mL). The product was isolated from the methylene chloride extraction of the acidic aqueous layer. The product was made basic by extraction with aqueous NaOH. The organic solution was concentrated, and the residue was distilled (150°-200° C., 0.10 mm) to afford 3.6 g of product.

後処理

  1. extractionThe product was made basic by extraction with aqueous NaOH
  2. concentrationThe organic solution was concentrated
  3. distillationthe residue was distilled (150°-200° C., 0.10 mm)

出典と根拠

ORDレコード
ord-2d5411438995407a8aed364ea93d54cb
出典データセット
uspto-grants-1990_01
特許番号
US04895951

反応ノート

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