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Ammonium Chloride → 3-Amino-3-[2-(4-octylphenyl)ethyl]hexane-1,6-diol

HRID 842261
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HRID 842261 반응식
C([O:4][CH2:5][CH2:6][C:7]([NH:31]C(=O)C)([CH2:15][CH2:16][C:17]1[CH:22]=[CH:21][C:20]([CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30])=[CH:19][CH:18]=1)[CH2:8][CH2:9][CH2:10][O:11]C(=O)C)(=O)C.O.[OH-].[Li+].[Cl-].[NH4+]>CO.O>[NH2:31][C:7]([CH2:15][CH2:16][C:17]1[CH:22]=[CH:21][C:20]([CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30])=[CH:19][CH:18]=1)([CH2:8][CH2:9][CH2:10][OH:11])[CH2:6][CH2:5][OH:4]
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참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 168937Lithium hydroxide, monohydrateHCID 10648237HCID 10648237, 화합물

생성물 1

HCID 158641333-Amino-3-[2-(4-octylphenyl)ethyl]hexane-1,6-diol수율 98.7%

시약·촉매·용매 1

HCID 22242641Methanol--water (1/1)용매

실험 절차

To a solution of 3-acetamido-6-acetoxy-3-[2-(4-octylphenyl)ethyl]hexyl acetate (400 mg) in methanol-water (1:1) (12 ml), lithium hydroxide monohydrate (360 mg) was added at room temperature and the mixture was refluxed under heating for 4 hours. After cooling, the mixture was neutralized with ammonium chloride and the solvent was distilled away under reduced pressure. The residue obtained was extracted with chloroform, the extract was washed with water and a saturated brine and dried over anhydrous magnesium sulfate. The solvent was distilled away to give the subject compound (290 mg) as a yellowish oily substance.

후처리

  1. temperaturethe mixture was refluxed
  2. temperatureunder heating for 4 hours
  3. temperatureAfter cooling
  4. distillationthe solvent was distilled away under reduced pressure
  5. customThe residue obtained
  6. extractionwas extracted with chloroform
  7. washthe extract was washed with water
  8. dry with materiala saturated brine and dried over anhydrous magnesium sulfate
  9. distillationThe solvent was distilled away

출처 및 근거

ORD 기록
ord-be5d4387163d42cbac5e23f09f2ce557
출처 데이터셋
uspto-grants-2002_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06372800B1

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