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Acetic Anhydride → HCID 86698039、化合物

HRID 518889
ノート
印刷プレビュー

反応式

HRID 518889 の反応式
[C:1](OC(=O)C)(=[O:3])C.[CH3:8][N:9]1[CH2:14][CH2:13][CH:12]([C:15]2[CH:21]=[CH:20][C:18]([NH2:19])=[C:17]([O:22][CH:23]([CH3:25])[CH3:24])[CH:16]=2)[CH2:11][CH2:10]1>C(O)=O>[CH3:8][N:9]1[CH2:14][CH2:13][CH:12]([C:15]2[CH:21]=[CH:20][C:18]([NH:19][CH:1]=[O:3])=[C:17]([O:22][CH:23]([CH3:25])[CH3:24])[CH:16]=2)[CH2:11][CH2:10]1
参加物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 7918Acetic AnhydrideHCID 683600014-(1-Methylpiperidin-4-yl)-2-(propan-2-yloxy)aniline

生成物 1

HCID 86698039HCID 86698039、化合物収率 74.9%

試薬・触媒・溶媒 1

HCID 284Formic Acid溶媒2 回

実験手順

A solution of 12.3 g of acetic anhydride is added slowly to 19 ml of formic acid at ambient temperature. After one hour of stirring, a solution of 6.0 g of 4-(1-methylpiperidin-4-yl)-2-(propan-2-yloxy)aniline in 28 ml of formic acid is added dropwise. The mixture is stirred at ambient temperature for 2 h and then concentrated under vacuum and taken up with water. The aqueous phase is neutralized with a saturated sodium bicarbonate solution and extracted three times with 100 ml of dichoromethane. The organic phases are dried over magnesium sulfate, filtered and concentrated under vacuum. The crude product is triturated with ethyl ether and the solid is filtered off, so as to obtain 5.0 g of N-[4-(1-methylpiperidin-4-yl)-2-(propan-2-yloxy)phenyl]formamide.

後処理

  1. stirringThe mixture is stirred at ambient temperature for 2 h
  2. concentrationconcentrated under vacuum
  3. extractionextracted three times with 100 ml of dichoromethane
  4. dry with materialThe organic phases are dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under vacuum
  7. customThe crude product is triturated with ethyl ether
  8. filtrationthe solid is filtered off

出典と根拠

ORDレコード
ord-5b8065186a884698bc84024d20283e35
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09115140B2

反応ノート

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