Water → Butyl 1,6-dihydro-6-oxo-3-pyridazinecarboxylate

HRID 840303노트

반응식

HRID 840303 반응식
[O:1]=[C:2]1[NH:7][N:6]=[C:5]([C:8]([OH:10])=[O:9])[CH:4]=[CH:3]1.S(=O)(=O)(O)O.O>C(OC(C)=O)CCC.C(O)CCC>[O:1]=[C:2]1[NH:7][N:6]=[C:5]([C:8]([O:10][CH2:2][CH2:3][CH2:4][CH3:5])=[O:9])[CH:4]=[CH:3]1

참가 물질

6

반응물 3

HCID 962WaterHCID 1118Sulfuric AcidHCID 3059706-Hydroxypyridazine-3-carboxylic Acid

생성물 1

HCID 12346430Butyl 1,6-dihydro-6-oxo-3-pyridazinecarboxylate수율 170.5%

시약·촉매·용매 2

HCID 2631-Butanol용매HCID 31272Butyl Acetate용매

실험 절차

A solution of 6-oxo-1,6-dihydropyridazine-3-carboxylic acid (British patent no. 856409) (52 g, 0.33 mol) in nBuOAc (80 ml) and butanol (80 ml) was treated with concentrated sulphuric acid (5 ml). The mixture was heated at reflux under a Dean-Stark trap. After 5 hours water production had ceased. The reaction was allowed to cool to ambient temperature and after standing overnight, the precipitate was filtered, washed with diethyl ether and dried to give butyl 6-oxo-1,6-dihydropyridazine-3-carboxylate as a white solid (55.2 g, 85%) m.p. 81-83° C.

후처리

  1. temperatureThe mixture was heated
  2. temperatureat reflux under a Dean-Stark trap
  3. filtrationthe precipitate was filtered
  4. washwashed with diethyl ether
  5. customdried

출처 및 근거

ORD 기록
ord-94d09b112ac748a396e5418bcc6a2711
출처 데이터셋
uspto-grants-2002_04
특허 번호
US06365603B1

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