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Water → HCID 23153447, 화합물

HRID 1712641
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HRID 1712641 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[N:7]1([C:11](=O)[CH2:12][N:13]2[CH2:18][CH2:17][N:16]([C:19](=O)[C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[CH2:15][CH2:14]2)[CH2:10][CH2:9][CH2:8]1.O.[OH-].[Na+]>O1CCCC1>[N:7]1([CH2:11][CH2:12][N:13]2[CH2:14][CH2:15][N:16]([CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[CH2:17][CH2:18]2)[CH2:8][CH2:9][CH2:10]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 23153146HCID 23153146, 화합물

생성물 1

HCID 23153447HCID 23153447, 화합물수율 104.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

Lithium aluminium hydride (405 mg) was suspended in tetrahydrofuran (10 ml) under a nitrogen atmosphere with stirring in an ice water bath, 1-(azetidin-1-yl)-2-(4-benzoylpiperazin-1-yl)ethanone (730 mg) and tetrahydrofuran (5 ml×3) was added thereto. The reaction mixture was stirred at 60° C. for 3 hours. The reaction mixture was allowed to cool down to room temperature, and water (0.4 ml), a 5N aqueous solution of sodium hydroxide (0.4 ml) and water (1.2 ml) were added thereto, followed by stirring for 13 hours. The insoluble matter in the reaction mixture was removed by filtration through celite, and washed with ethyl acetate (100 ml). The solvent was distilled off under reduced pressure to give a crude product of the title compound (687 mg) as a pale yellow oil.

후처리

  1. stirringThe reaction mixture was stirred at 60° C. for 3 hours
  2. stirringby stirring for 13 hours
  3. customThe insoluble matter in the reaction mixture was removed by filtration through celite
  4. washwashed with ethyl acetate (100 ml)
  5. distillationThe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-b11572b74b2f4483b041f0f82cfa2fcc
출처 데이터셋
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07790885B2

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