Ethanol → HCID 178434443、化合物

HRID 643977ノート

反応式

HRID 643977 の反応式
C([O-])(=O)C.[Na+].[NH2:6][NH:7][C:8]([NH2:10])=[S:9].C(O)C.[CH3:14][C:15]1[C:23]2[C:18](=[N:19][CH:20]=[C:21]([CH:24]=O)[CH:22]=2)[NH:17][N:16]=1>O>[CH3:14][C:15]1[C:23]2[C:18](=[N:19][CH:20]=[C:21]([CH:24]=[N:6][NH:7][C:8]([NH2:10])=[S:9])[CH:22]=2)[NH:17][N:16]=1

参加物

6

反応物 4

HCID 702EthanolHCID 517045Sodium AcetateHCID 2723789ThiosemicarbazideHCID 178434462HCID 178434462、化合物

生成物 1

HCID 178434443HCID 178434443、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

Sodium acetate (166 mg, 2.02 mmol), thiosemicarbazide (333 mg, 3.66 mmol), 100 ml ethanol and 2 ml distilled water were charged into a 250 ml round bottom flask. The resulting suspension was heated to 80° C. until it becomes a clear solution. The reaction was then cooled down to room temperature and the resulting mixture was added into a 250 ml round bottom flask containing 3-methyl-1H-pyrazolo[3,4-b]pyridine-5-carbaldehyde (333 mg, 2.1 mmol). After the addition, the resulting mixture was heated to 80° C. for 16 hours. The mixture was cooled to room temperature and solid was precipitated out. The solid was filtered off and washed with ether (50 ml). The product (500 mg, y=95%) was used directly for the next step without further purification.

後処理

  1. additionwere charged into a 250 ml round bottom flask
  2. temperatureThe reaction was then cooled down to room temperature
  3. additionthe resulting mixture was added into a 250 ml round bottom flask
  4. additionAfter the addition
  5. temperaturethe resulting mixture was heated to 80° C. for 16 hours
  6. temperatureThe mixture was cooled to room temperature
  7. customsolid was precipitated out
  8. filtrationThe solid was filtered off
  9. washwashed with ether (50 ml)
  10. customThe product (500 mg, y=95%) was used directly for the next step without further purification

出典と根拠

ORDレコード
ord-58621cb93db648ffa933811283c99af1
出典データセット
uspto-grants-2010_04
特許番号
US07700636B2

反応ノート

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