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

HRID 1731412ノート

反応式

HRID 1731412 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0f6d5a9c9d604a8aacbafa64b7916564
出典データセット
uspto-grants-1986_11
特許番号
US04621142

反応ノート

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