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Acetic Anhydride → HCID 86698039, 화합물

HRID 518889
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HRID 518889 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 683600014-(1-Methylpiperidin-4-yl)-2-(propan-2-yloxy)aniline

생성물 1

HCID 86698039HCID 86698039, 화합물수율 74.9%

시약·촉매·용매 1

HCID 284Formic Acid용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5b8065186a884698bc84024d20283e35
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09115140B2

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