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

HRID 330364노트

반응식

HRID 330364 반응식
[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]

참가 물질

5

반응물 4

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

생성물 1

HCID 578921Pyridine-2,3-dicarboxamide

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-664d61f0a549455c90c7133988cca0cf
출처 데이터셋
uspto-grants-1990_01
특허 번호
US04895951

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