Water → HCID 140606546、化合物

HRID 920947ノート

反応式

HRID 920947 の反応式
[Cl:1][C:2]1[CH:12]=[N:11][CH:10]=[C:9]([CH:13]=O)[C:3]=1[C:4]([O:6][CH2:7][CH3:8])=[O:5].[C:15]([NH:18][NH2:19])(=[O:17])[CH3:16].C(Cl)Cl.O>C(O)C>[C:15]([NH:18]/[N:19]=[CH:13]/[C:9]1[CH:10]=[N:11][CH:12]=[C:2]([Cl:1])[C:3]=1[C:4]([O:6][CH2:7][CH3:8])=[O:5])(=[O:17])[CH3:16]

参加物

6

反応物 4

HCID 962WaterHCID 6344DichloromethaneHCID 14039AcetohydrazideHCID 86683163HCID 86683163、化合物

生成物 1

HCID 140606546HCID 140606546、化合物収率 8.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To ethyl 3-chloro-5-formylisonicotinate (2 g, 9.36 mmol) in 60 mL of ethanol was added acetohydrazide (0.832 g, 11.24 mmol) at room temperature. The reaction mixture was stirred for 2 h. Then, the reaction mixture was mixed with DCM and water. The organic phase was washed with brine, dried and concentrated. The crude title compound was purified by chromatography (eluent: DCM/methanol) to give 220 mg (8.7%) of the title compound as orange oil.

後処理

  1. washThe organic phase was washed with brine
  2. customdried
  3. concentrationconcentrated
  4. customThe crude title compound was purified by chromatography (eluent: DCM/methanol)

出典と根拠

ORDレコード
ord-86379242d9634b108bdb63c8688bfc12
出典データセット
uspto-grants-2016_03
特許番号
US09273068B2

反応ノート

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