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Ammonium Hydroxide → Ethyl [4-(methoxymethyl)piperidin-4-yl]phenylcarbamate

HRID 1973848
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HRID 1973848 반응식
[CH2:1]([O:3][C:4]([N:6]([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)[C:7]1([CH2:23][O:24][CH3:25])[CH2:12][CH2:11][N:10](C(OCC2C=CC=CC=2)=O)[CH2:9][CH2:8]1)=[O:5])[CH3:2].[OH-].[NH4+].[H][H]>[Pd].CO>[CH3:25][O:24][CH2:23][C:7]1([N:6]([C:26]2[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=2)[C:4](=[O:5])[O:3][CH2:1][CH3:2])[CH2:8][CH2:9][NH:10][CH2:11][CH2:12]1
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참가 물질

6

반응물 3

HCID 14923Ammonium HydroxideHCID 53960004HCID 53960004, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 54010374Ethyl [4-(methoxymethyl)piperidin-4-yl]phenylcarbamate수율 81.4%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol
용매

실험 절차

A solution of 14.2 parts of (phenylmethyl) 4-[(ethoxycarbonyl)phenylamino]-4-(methoxymethyl)-1-piperidinecarboxylate and 1.8 parts of ammonium hydroxide in 120 parts of methanol is hydrogenated at normal pressure and at room temperature with 4 parts of palladium-on-charcoal catalyst 10%. After the calculated amount of hydrogen is taken up, the catalyst is filtered off and the filtrate is evaporated. The residue is dissolved in 75 parts of trichloromethane. The solution is washed twice with water, dried, filtered and evaporated, yielding 7.9 parts (81.4%) of ethyl [4-(methoxymethyl)-4-piperidinyl]phenylcarbamate as a residue.

후처리

  1. filtrationthe catalyst is filtered off
  2. customthe filtrate is evaporated
  3. dissolutionThe residue is dissolved in 75 parts of trichloromethane
  4. washThe solution is washed twice with water
  5. customdried
  6. filtrationfiltered
  7. customevaporated

출처 및 근거

ORD 기록
ord-c1fe4ae7fd5a4906b81f60f1ab6eb24a
출처 데이터셋
uspto-grants-1976_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03998834

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