Ethyl Acetate → HCID 10435214, 화합물

HRID 370662

반응식

HRID 370662 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([O:14][C:15]1[CH:20]=[CH:19][C:18]([C:21](=[O:42])[CH2:22][N:23]2[CH2:28][CH2:27][N:26]([CH:29]([C:36]3[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=3)[C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=3)[CH2:25][CH2:24]2)=[CH:17][CH:16]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.C(OCC)(=O)C.[Cl-].[NH4+]>O1CCCC1>[CH2:7]([O:14][C:15]1[CH:16]=[CH:17][C:18]([CH:21]([OH:42])[CH2:22][N:23]2[CH2:24][CH2:25][N:26]([CH:29]([C:30]3[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=3)[C:36]3[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=3)[CH2:27][CH2:28]2)=[CH:19][CH:20]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

참가 물질

6

반응물 4

HCID 8857Ethyl Acetate2회HCID 25517Ammonium ChlorideHCID 103227601-(4-Benzyloxyphenyl)-2-(4-diphenylmethylpiperazinyl)ethanoneHCID 21226445Aluminium lithium hydride

생성물 1

HCID 10435214HCID 10435214, 화합물수율 79%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

In 24 ml of tetrahydrofuran was suspended 0.60 g (16 mmol) of lithium aluminum hydride, to which a suspension consisting of 24 ml of tetrahydrofuran and 3.0 g (6.3 mmol) of 1-(4-benzyloxyphenyl)-2-(4-diphenylmethylpiperazinyl)ethanone was added portionwise under ice-cooled conditions. After being stirred for 0.5 hour, the resultant mixture was added dropwise with 5 ml of ethyl acetate, followed by further addition of 50 ml of ethyl acetate. The thus prepared solution was poured into an aqueous solution of ammonium chloride, and the organic layer was separated. The organic layer was washed twice with saturated saline and then dried over anhydrous sodium sulfate. The solvent was removed, and the residue was recrystallized from a mixed solvent of ethanol and chloroform to give 2.37 g of 1-(4-benzyloxyphenyl)-2-(4-diphenylmethylpiperazinyl)ethanol (yield: 79%).

후처리

  1. additionwas added portionwise under ice-
  2. temperaturecooled conditions
  3. customthe organic layer was separated
  4. washThe organic layer was washed twice with saturated saline
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe solvent was removed
  7. customthe residue was recrystallized from a mixed solvent of ethanol and chloroform

출처 및 근거

ORD 기록
ord-63c838f4feed4e71ab42cffecb96d306
출처 데이터셋
uspto-grants-1985_07
특허 번호
US04528194

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