Triethylamine → HCID 178423916、化合物

HRID 1368658

反応式

HRID 1368658 の反応式
C(O[C:4](=[O:14])[CH:5]([C:12]#[N:13])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)C.Cl.Cl.[CH2:17]([NH:24][NH2:25])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.[CH2:26](N(CC)CC)C>C(O)C.C(OCC)(=O)C>[NH2:13][C:12]1[N:24]([CH2:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[N:25]=[C:4]([OH:14])[C:5]=1[C:6]1[CH:7]=[CH:8][C:9]([CH3:26])=[CH:10][CH:11]=1

参加物

6

反応物 3

HCID 8471TriethylamineHCID 95298Ethyl phenylcyanoacetateHCID 146540Benzylhydrazine dihydrochloride

生成物 1

HCID 178423916HCID 178423916、化合物収率 20%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a stirring suspension of ethyl-2-cyano-2-phenylacetate (10.34 g) and benzylhydrazine dihydrochloride (14.87 g) in ethanol (200 ml) at room temperature was added triethylamine (21.27 ml). The reaction mixture was heated to reflux for 24 hours. The solvent was removed under reduced pressure to yield the crude material as a brown oil. This was re-dissolved in ethyl acetate (100 ml) and washed with water (2×75 ml), then dried (MgSO4) and the solvent removed in vacuo to yield a pale brown oil. This was recrystallised from methanol to yield the title product as pale yellow crystals (2.5 g, ca. 20%)

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 24 hours
  3. customThe solvent was removed under reduced pressure
  4. customto yield the crude material as a brown oil
  5. washwashed with water (2×75 ml)
  6. dry with materialdried (MgSO4)
  7. customthe solvent removed in vacuo
  8. customto yield a pale brown oil
  9. customThis was recrystallised from methanol

出典と根拠

ORDレコード
ord-e9cea2c5de7443668f7e48ae77ac952e
出典データセット
uspto-grants-2003_06
特許番号
US06573270B1

関連ノート

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