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Sulfuric Acid → HCID 131719371、化合物

HRID 1378920
ノート
印刷プレビュー

反応式

HRID 1378920 の反応式
C(OC(=O)[C:5]1[CH:10]=[CH:9][CH:8]=[N:7][C:6]=1[CH:11]1[CH:16]=[CH:15][CH2:14][N:13](C(OCC)=O)[N:12]1[C:22]([O:24]CC)=O)C.OS(O)(=O)=O.C([O-])([O-])=O.[Na+].[Na+]>O>[NH:13]1[CH2:14][CH2:15][CH:16]=[C:11]2[C:6]3[N:7]=[CH:8][CH:9]=[CH:10][C:5]=3[C:22](=[O:24])[N:12]12
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 10340Sodium CarbonateHCID 53698348HCID 53698348、化合物

生成物 1

HCID 131719371HCID 131719371、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

6.6 g of 2-(1,2-diethoxycarbonyl-1,2,3,6-tetrahydropyridazin-3-yl)nicotinic acid ethyl ester are mixed with 15 ml water and 60 ml of H2SO4 added with cooling. The reaction mixture is heated under nitrogen to 120° over 1 hr in a hot oil bath. The mixture is slowly poured into 125 g Na2CO3 and 250 g of ice and 125 ml of water. The alkaline mixture is filtered through celite and repeatedly extracted with ethylacetate (8×100 ml) and the extracts dried over MgSO4. After filtration the solvent is removed by evaporation under vacuum to yield the title compound which is recrystalized from CH3CN.

後処理

  1. additionadded
  2. temperaturewith cooling
  3. temperatureThe reaction mixture is heated under nitrogen to 120° over 1 hr in a hot oil bath
  4. filtrationThe alkaline mixture is filtered through celite
  5. extractionrepeatedly extracted with ethylacetate (8×100 ml)
  6. dry with materialthe extracts dried over MgSO4
  7. filtrationAfter filtration the solvent
  8. customis removed by evaporation under vacuum

出典と根拠

ORDレコード
ord-1ff5aa96347d46ff849dc5ef443eeecf
出典データセット
uspto-grants-1997_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05670456

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート