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

HRID 635457
ノート
印刷プレビュー

反応式

HRID 635457 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 168937Lithium hydroxide, monohydrateHCID 10648237HCID 10648237、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 22242641Methanol--water (1/1)溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0aae1ccb26ac4ce6b39ec001ddb1ec3c
出典データセット
uspto-grants-2001_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06187821B1

反応ノート

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