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

HRID 330363노트

반응식

HRID 330363 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 578921Pyridine-2,3-dicarboxamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-2d5411438995407a8aed364ea93d54cb
출처 데이터셋
uspto-grants-1990_01
특허 번호
US04895951

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