Water → HCID 19778888, 화합물

HRID 2081916노트

반응식

HRID 2081916 반응식
C(N(CC)CC)C.Cl.Cl.[CH3:10][O:11][C:12](=[NH:17])[CH:13]=[C:14]([NH2:16])[CH3:15].[Cl-].[CH2:19]([O:21][C:22](=[O:26])[C:23](O)=O)[CH3:20].O>ClCCl>[CH3:10][O:11][C:12]1[CH:13]=[C:14]([CH3:15])[N:16]=[C:23]([C:22]([O:21][CH2:19][CH3:20])=[O:26])[N:17]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 23618337Oxalic acid monoethylester chlorideHCID 86745111Methyl-3-amino-2-butenimidate dihydrochloride

생성물 1

HCID 19778888HCID 19778888, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

182 ml of triethylamine in 50 ml of dichloromethane are added dropwise at -30° C. to a stirred suspension of 70.2 g of methyl-3-amino-2-butenimidate dihydrochloride in 350 ml of dichloromethane. Stirring is continued for 0.5 hour at this temperature, and 42 ml of oxalic acid ethyl ester chloride are then added dropwise. Stirring is continued for 1 hour at -30° C., and the mixture is allowed to come to room temperature in the course of 12 hours. The organic phase is stirred several times with water, dried over Na2SO4 and concentrated. After filtration over silica gel (eluent: CH2Cl2), the residue is distilled in vacuo. This gives 51.5 g of ethyl 4-methoxy-6-methylpyrimidine-2-carboxylate of boiling point 105°-115° C./0.05 mbar.

후처리

  1. additionare then added dropwise
  2. stirringStirring
  3. customto come to room temperature in the course of 12 hours
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated
  6. filtrationAfter filtration over silica gel (eluent: CH2Cl2)
  7. distillationthe residue is distilled in vacuo

출처 및 근거

ORD 기록
ord-e35b5996810e43fba0f7b56516b19f8d
출처 데이터셋
uspto-grants-1993_02
특허 번호
US05186736

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