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Benzoyl chloride → HCID 18700007、化合物

HRID 2288615
ノート
印刷プレビュー

反応式

HRID 2288615 の反応式
[C:1]([Cl:9])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH2:10][C:11]1[O:15][C:14]([C:16]2[S:20][C:19]([CH2:21][N:22]3[CH2:28][CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]3)=[CH:18][CH:17]=2)=[N:13][N:12]=1>N1C=CC=CC=1>[ClH:9].[N:22]1([CH2:21][C:19]2[S:20][C:16]([C:14]3[O:15][C:11]([NH:10][C:1](=[O:8])[C:2]4[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=4)=[N:12][N:13]=3)=[CH:17][CH:18]=2)[CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 7412Benzoyl chlorideHCID 18699937HCID 18699937、化合物

生成物 1

HCID 18700007HCID 18700007、化合物収率 57.5%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
80 °C

実験手順

1.8 ml (15.0 mmol) of benzoyl chloride was added to 15 ml of pyridine solution containing 278 mg (1.0 mmol) of the compound of Example 43, and the mixture was stirred at 80° C. for 10 days. The reaction solution was concentrated under a reduced pressure, chloroform was added to the resulting residue, followed by washing with water and drying over anhydrous magnesium sulfate. The solvent was evaporated, the resulting residue was purified by a silica gel column chromatography. Then, the resulting crude crystals were recrystallized from ethanol-diisopropyl ether to give 241 mg of the title compound.

後処理

  1. concentrationThe reaction solution was concentrated under a reduced pressure, chloroform
  2. additionwas added to the resulting residue
  3. washby washing with water
  4. dry with materialdrying over anhydrous magnesium sulfate
  5. customThe solvent was evaporated
  6. customthe resulting residue was purified by a silica gel column chromatography
  7. customThen, the resulting crude crystals were recrystallized from ethanol-diisopropyl ether

出典と根拠

ORDレコード
ord-d9986c1c58074a428f8f42c2e6dd893c
出典データセット
uspto-grants-2000_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06090804

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート