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

HRID 330361ノート

反応式

HRID 330361 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]([NH:13]C(C)(C)CC(C)(C)C)=[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 3524332-chloro-N-(1,1,3,3-tetramethylbutyl)acetamide

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 4 was prepared according to the general procedure described in Example 8 using 2-(aminomethyl)pyridine (0.011 mol), 2-chloro-N-(1,1,3,3,-tetramethylbutyl)acetamide (0.033 mol), diisopropylethylamine (0.025 mol) and dimethoxyethane (25 mL). The product was isolated from the methylene chloride extraction of the acidic aqueous layer. The product was made basic by extraction of the methylene chloride solution with aqueous NaOH. The methylene chloride solution was concentrated, and the residue was distilled (150° C., 0.03 mm) to afford 3.7 g of pure product.

後処理

  1. extractionThe product was made basic by extraction of the methylene chloride solution with aqueous NaOH
  2. concentrationThe methylene chloride solution was concentrated
  3. distillationthe residue was distilled (150° C., 0.03 mm)

出典と根拠

ORDレコード
ord-31842623b17d4ff58481920f0a65a183
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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