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Acetyl chloride → HCID 10517454、化合物

HRID 1383619
ノート
印刷プレビュー

反応式

HRID 1383619 の反応式
[OH:1][C@H:2]1[CH2:16][CH:15]=[C:14]2[C@:4]([CH3:17])([CH2:5][C:6]3[C:7](=[CH:13]2)[O:8][C:9](=[O:12])[C:10]=3[CH3:11])[C@H:3]1[CH3:18].[C:19](Cl)(=[O:21])[CH3:20].S([O-])(O)(=O)=O.[K+]>N1C=CC=CC=1>[C:19]([O:1][C@H:2]1[CH2:16][CH:15]=[C:14]2[C@:4]([CH3:17])([CH2:5][C:6]3[C:7](=[CH:13]2)[O:8][C:9](=[O:12])[C:10]=3[CH3:11])[C@H:3]1[CH3:18])(=[O:21])[CH3:20]
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

5

反応物 3

HCID 6367Acetyl chlorideHCID 516920Potassium bisulfateHCID 10514571HCID 10514571、化合物

生成物 1

HCID 10517454HCID 10517454、化合物収率 80%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
25 °C

実験手順

The compound prepared in Example B1 (in the general formula (II), R3=H, R4=CH3, and R5=H) (50 mg, 0.20 mmol) was dissolved in pyridine (5 ml), acetyl chloride (80 mg, 0.70 mmol) was added thereto, and the mixture was stirred at 25° C. for one hr. A 15% aqueous potassium hydrogensulfate solution was added to the reaction solution, followed by extraction with methylene chloride. The organic layer was washed with saturated saline and dried over magnesium sulfate, and the solvent was removed by distillation under reduced pressure. The residue was purified by column chromatography on silica gel (hexane:ethyl acetate=3:1) to give the title compound (55 mg, 80%).

後処理

  1. extractionfollowed by extraction with methylene chloride
  2. washThe organic layer was washed with saturated saline
  3. dry with materialdried over magnesium sulfate
  4. customthe solvent was removed by distillation under reduced pressure
  5. customThe residue was purified by column chromatography on silica gel (hexane:ethyl acetate=3:1)

出典と根拠

ORDレコード
ord-f35c0377f91243f1a1e5a65a099dcd23
出典データセット
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06255339B1

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