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

HRID 330361노트

반응식

HRID 330361 반응식
[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]

참가 물질

6

반응물 4

HCID 80711,2-DimethoxyethaneHCID 195092-PyridinemethanamineHCID 81531DiisopropylethylamineHCID 3524332-chloro-N-(1,1,3,3-tetramethylbutyl)acetamide

생성물 1

HCID 578921Pyridine-2,3-dicarboxamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-31842623b17d4ff58481920f0a65a183
출처 데이터셋
uspto-grants-1990_01
특허 번호
US04895951

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