Acetohydrazide → HCID 57650585、化合物

HRID 2063476ノート

反応式

HRID 2063476 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C@@H:8]([NH:10][C:11]([C@H:13]2[CH2:17][CH2:16][CH2:15][N:14]2[C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])=S)[CH3:9])=[CH:4][CH:3]=1.[C:25]([NH:28][NH2:29])(=O)[CH3:26]>C(#N)C.C([O-])(=O)C.[Hg+2].C([O-])(=O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C@@H:8]([N:10]2[C:25]([CH3:26])=[N:28][N:29]=[C:11]2[C@H:13]2[CH2:17][CH2:16][CH2:15][N:14]2[C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH3:9])=[CH:4][CH:3]=1

参加物

5

反応物 2

HCID 14039AcetohydrazideHCID 57650584HCID 57650584、化合物

生成物 1

HCID 57650585HCID 57650585、化合物

試薬・触媒・溶媒 2

HCID 15337Mercuric acetate触媒HCID 6342Acetonitrile溶媒

実験手順

To a mixture of the product of Step B (1.7 g, 4.6 mmol) and acetic hydrazide (0.76 g, 9.2 mmol) in 30 ml acetonitile was added mercury (II) acetate (2.2 g, 6.9 mmol) and the mixture was stirred at room temperature for overnight. The mixture was filtered over a Celite-fritted funnel and washed with more acetonitrile. The filtrate was concentrated in vacuo. Run wash column yield the desired product containing minor impurities (1.3 g, 72%), was used in the next step without further purification.

後処理

  1. filtrationThe mixture was filtered over a Celite-fritted funnel
  2. washwashed with more acetonitrile
  3. concentrationThe filtrate was concentrated in vacuo
  4. washRun wash column

出典と根拠

ORDレコード
ord-c239f37011df4052a4fc9114b05adc20
出典データセット
uspto-grants-2012_10
特許番号
US08288371B2

反応ノート

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