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Acetic Anhydride → HCID 21409851, 화합물

HRID 1283536
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HRID 1283536 반응식
C(O[C:5](=[O:7])C)(=O)C.[CH3:8][NH:9][CH2:10][C:11]1([N:17]2[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]2)[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1>C(O)=O>[CH:5]([N:9]([CH2:10][C:11]1([N:17]2[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]2)[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1)[CH3:8])=[O:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 21409890N-Methyl-1-[1-(piperidin-1-yl)cyclohexyl]methanamine

생성물 1

HCID 21409851HCID 21409851, 화합물

시약·촉매·용매 1

HCID 284Formic Acid용매2회

실험 절차

Formic acid 98/100% (13.8 g. 0.3 mole) and acetic anhydride (30.6 g. 0.3 mole) were mixed without cooling and kept at room temp. for 1 hr. 1-(1-methylaminomethylcyclohexyl) piperidine (4.2 g. 0.02 mole) was dissolved in formic acid (15 ml) and the formylating agent (25 ml) added slowly. This produced effervescence and a rise in temp. to 60°. The mixture was allowed to stand at room temp. overnight and the solvents then evaporated under reduced pressure to yield a viscous, amber oil (3.79 g. 80%) which crystallised on cooling and gave colourless prisms of 1-(N-formyl-1-methylaminomethylcyclohexyl) piperidine m.p. 94° (from light petroleum b.p. 60°-80°).

후처리

  1. temperaturewithout cooling
  2. additionthe formylating agent (25 ml) added slowly
  3. customto 60°
  4. waitto stand at room temp. overnight
  5. customthe solvents then evaporated under reduced pressure
  6. customto yield a viscous, amber oil (3.79 g. 80%) which
  7. customcrystallised
  8. temperatureon cooling

출처 및 근거

ORD 기록
ord-4e1fb03640f8438e9814c2a3df7c9e8f
출처 데이터셋
uspto-grants-1976_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03975443

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