Hydrazine → 1-[[3-(3-Aminopropoxy)phenyl]carbonyl]piperidine

HRID 1731412노트

반응식

HRID 1731412 반응식
O=C1C2C(=CC=CC=2)C(=O)[N:3]1[CH2:12][CH2:13][CH2:14][O:15][C:16]1[CH:17]=[C:18]([CH:27]=[CH:28][CH:29]=1)[C:19]([N:21]1[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]1)=[O:20].NN>C(O)C>[NH2:3][CH2:12][CH2:13][CH2:14][O:15][C:16]1[CH:17]=[C:18]([C:19]([N:21]2[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]2)=[O:20])[CH:27]=[CH:28][CH:29]=1

참가 물질

4

반응물 2

HCID 9321HydrazineHCID 137325571-[3-[3-(1,3-dihydro-1,3-dioxo-2H-isoindol-2-yl)propoxy]benzoyl]piperidine

생성물 1

HCID 137325581-[[3-(3-Aminopropoxy)phenyl]carbonyl]piperidine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a warm solution of 0.5 g. of 1-[3-[3-(1,3-dihydro-1,3-dioxo-2H-isoindol-2-yl)propoxy]benzoyl]piperidine in 20 ml. of absolute ethanol is added 1 ml. of hydrazine. The mixture is stirred at room temperature for 1 hour and is filtered. The filtrate is allowed to stand at room temperature for 18 hours and again is filtered. The filtrate is evaporated in a rotary evaporator and the residue is partitioned between 50 ml. of ether and 50 ml. of water. The ether layer is dried over magnesium sulfate, is filtered and is evaporated to give 80 mg. of oil. The oil is purified by HPLC using 1-Silica Prep Pac (Waters) and a combination of methanol, ethyl acetate and 1% triethylamine to give the analytical sample.

후처리

  1. filtrationis filtered
  2. waitto stand at room temperature for 18 hours
  3. filtrationagain is filtered
  4. customThe filtrate is evaporated in a rotary evaporator
  5. customthe residue is partitioned between 50 ml
  6. dry with materialThe ether layer is dried over magnesium sulfate
  7. filtrationis filtered
  8. customis evaporated
  9. customto give 80 mg
  10. customThe oil is purified by HPLC
  11. customa combination of methanol, ethyl acetate and 1% triethylamine to give the analytical sample

출처 및 근거

ORD 기록
ord-0f6d5a9c9d604a8aacbafa64b7916564
출처 데이터셋
uspto-grants-1986_11
특허 번호
US04621142

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