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Sodium Hydroxide → HCID 19791670、化合物

HRID 1655323
ノート
印刷プレビュー

反応式

HRID 1655323 の反応式
N[CH:2]([CH2:11][CH2:12][CH:13]([CH3:15])[CH3:14])[CH:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)[OH:4].[Cl:16][CH2:17][CH2:18][N:19]1[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]1.[OH-].[Na+]>O>[ClH:16].[ClH:16].[CH3:14][CH:13]([CH3:15])[CH2:12][CH2:11][CH:2]([CH2:17][CH2:18][N:19]1[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]1)[CH:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)[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 14798Sodium HydroxideHCID 748271-(2-Chloroethyl)piperidineHCID 13671865HCID 13671865、化合物

生成物 1

HCID 19791670HCID 19791670、化合物収率 36.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of (1RS,2SR)-2-amino-5-methyl-1-phenylhexan-1-ol (1.04 g, 5 mmol) and 1-(2-chloroethyl)piperidine (0.74 g, 5 mmol) was melted at 70° C. in a nitrogen atmosphere. The mixture was then heated at 110° to 120° C. for 3 hours. After being cooled, the reaction mixture was dissolved in water. The solution was basified with 2N-NaOH and then extracted with ether. The ethereal extract was washed twice with water and once with brine, dried over anhydrous sodium sulfate and then evaporated under reduced pressure. The residue was dissolved in acetone (20 ml), followed by addition of concentrated hydrochloric acid (0.74 ml). Precipitated crystals were collected by filtration and washed with acetone. The crystals were recrystallized from ethanol (10 ml)-ether (2 ml) to obtain 0.34 g of the title compound as white crystals (yield: 17%).

後処理

  1. temperatureThe mixture was then heated at 110° to 120° C. for 3 hours
  2. temperatureAfter being cooled
  3. extractionextracted with ether
  4. extractionThe ethereal extract
  5. washwas washed twice with water and once with brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. customevaporated under reduced pressure
  8. dissolutionThe residue was dissolved in acetone (20 ml)
  9. additionfollowed by addition of concentrated hydrochloric acid (0.74 ml)
  10. customPrecipitated crystals
  11. filtrationwere collected by filtration
  12. washwashed with acetone
  13. customThe crystals were recrystallized from ethanol (10 ml)-ether (2 ml)

出典と根拠

ORDレコード
ord-c85db47876a64a3e84d94fb90f4fdc17
出典データセット
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05250546

反応ノート

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