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

HRID 330364ノート

反応式

HRID 330364 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](C(C)C)C(C)C)=[O:12].C(N(C(C)C)CC)(C)C.C(COC)[O:30]C>>[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:30]

参加物

5

反応物 4

HCID 80711,2-DimethoxyethaneHCID 195092-PyridinemethanamineHCID 81531DiisopropylethylamineHCID 1390132-chloro-N,N-bis(propan-2-yl)acetamide

生成物 1

HCID 578921Pyridine-2,3-dicarboxamide

実験手順

Pyridine diamide 7 was prepared according to the general procedure described in Example 8 using 2-(aminomethyl)pyridine (0.013 mol), 2-chloro-N,N-diisopropylacetamide (0.038 mol), diisopropylethylamine (0.038 mol) and dimethoxyethane (25 mL). The product was isolated from both the methylene chloride extraction of the acidic aqueous layer and the heptane extraction of the basic layer in about equal amounts. Mass spectral analysis of the two layers showed the material in the heptane layer to be of greater purity. The residue from the heptane layer was distilled (150° C., 0.05 mm) to afford 2.2 g of product.

後処理

  1. customThe product was isolated from both
  2. extractionthe methylene chloride extraction of the acidic aqueous layer
  3. extractionthe heptane extraction of the basic layer in about equal amounts
  4. distillationThe residue from the heptane layer was distilled (150° C., 0.05 mm)

出典と根拠

ORDレコード
ord-664d61f0a549455c90c7133988cca0cf
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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