Ammonium Chloride → HCID 22272787, 화합물

HRID 1064798노트

반응식

HRID 1064798 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([NH:14][C:15](=O)[CH2:16][N:17]1[CH2:22][CH2:21][N:20]([CH2:23][CH2:24][CH2:25][OH:26])[CH2:19][CH2:18]1)[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13].[Cl-].[NH4+]>C1COCC1>[CH2:7]([NH:14][CH2:15][CH2:16][N:17]1[CH2:18][CH2:19][N:20]([CH2:23][CH2:24][CH2:25][OH:26])[CH2:21][CH2:22]1)[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13]

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 21226445Aluminium lithium hydrideHCID 22272678HCID 22272678, 화합물

생성물 1

HCID 22272787HCID 22272787, 화합물수율 41.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Lithium aluminum hydride (380 mg, 10 mmol) was added to a solution of this amide (1.50 g, 5.0 mmol) in THF (50 ml) with ice-cooling and stirring and the mixture was returned to room temperature and stirred for 15 minutes and then heated to reflux for 2 hours. Under ice-cooling and stirring, a saturated ammonium chloride solution was gradually added thereto until the reaction solution became turbid, the separated matters were filtered off through celite, the filtrate was dried over anhydrous sodium carbonate and the solvent was evaporated therefrom. The resulting residue was purified by a silica gel column chromatography (75 g of silica gel; developing solvent, ammonia-saturated methanol:chloroform=1:20) to provide 586 mg (yield 41%) of 3-[4-(2-heptylaminoethyl)piperazin-1-yl]propanol as colorless oil.

후처리

  1. temperaturecooling
  2. customwas returned to room temperature
  3. stirringstirred for 15 minutes
  4. temperatureheated
  5. temperatureto reflux for 2 hours
  6. temperatureUnder ice-cooling
  7. stirringstirring
  8. filtrationthe separated matters were filtered off through celite
  9. dry with materialthe filtrate was dried over anhydrous sodium carbonate
  10. customthe solvent was evaporated
  11. customThe resulting residue was purified by a silica gel column chromatography (75 g of silica gel; developing solvent, ammonia-saturated methanol:chloroform=1:20)

출처 및 근거

ORD 기록
ord-90fa2867c31b470c98639c8a607aa2a1
출처 데이터셋
uspto-grants-2005_11
특허 번호
US06969711B2

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