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

HRID 840303

反応式

HRID 840303 の反応式
[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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 2631-Butanol溶媒HCID 31272Butyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-94d09b112ac748a396e5418bcc6a2711
出典データセット
uspto-grants-2002_04
特許番号
US06365603B1

関連ノート

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