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3-Chloropropylamine → (2R,3R,4R,5S)-3,4,5-tris(benzyloxy)-2-[(benzyloxy)methyl]-1-(3-chloropropyl)piperidine

HRID 1747014
ノート
印刷プレビュー

反応式

HRID 1747014 の反応式
[CH2:1]([O:8][C@H:9]([C@@H:12]([O:33][CH2:34][C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1)[C@H:13]([O:25][CH2:26][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)[C:14](=O)[CH2:15][O:16][CH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[CH:10]=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl:41][CH2:42][CH2:43][CH2:44][NH2:45].[BH3-]C#N.[Na+]>CO>[CH2:26]([O:25][C@H:13]1[C@H:12]([O:33][CH2:34][C:35]2[CH:36]=[CH:37][CH:38]=[CH:39][CH:40]=2)[C@@H:9]([O:8][CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[CH2:10][N:45]([CH2:44][CH2:43][CH2:42][Cl:41])[C@@H:14]1[CH2:15][O:16][CH2:17][C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1)[C:27]1[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=1
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 846293-ChloropropylamineHCID 5003444Sodium cyanoborohydrideHCID 11103493(2R,3R,4S)-2,3,4,6-tetrakis(benzyloxy)-5-oxohexanal

生成物 1

HCID 118407745(2R,3R,4R,5S)-3,4,5-tris(benzyloxy)-2-[(benzyloxy)methyl]-1-(3-chloropropyl)piperidine収率 36%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a stirred suspension of crude (2R,3R,4S)-2,3,4,6-tetrakis(benzyloxy)-5-oxohexanal 3 (20 g, 37.13 mmol) in MeOH (400 mL) were added 3-chloro propylamine (47 g, 743 mmol) at 0° C. and activated molecular sieves (100 g) and the reaction mixture was stirred at room temperature for 20 min. Then the reaction mixture was cooled to 0° C. and solid NaBH3CN (9.33 g, 148.5 mmol) was added to the reaction mixture and stirred at same temperature for 1 h. Then the reaction mixture was stirred at room temperature for 20 h. After removal of the molecular sieves through celite pad, the filtrate was concentrated under reduced pressure. The crude mass was dissolved in ethyl acetate (250 mL) and organic part was washed with saturated solution of NaHCO3 (100 mL), dried over Na2SO4 and concentrated under reduced pressure to get crude which was purified by column chromatography using 100-200 mesh silica gel and eluting with 8% EtOAc/hexane to afford (2R,3R,4R,5S)-3,4,5-tris(benzyloxy)-2-[(benzyloxy)methyl]-1-(3-chloropropyl)piperidine 4 (8.0 g, 36%) as white solid.

後処理

  1. temperatureThen the reaction mixture was cooled to 0° C.
  2. stirringstirred at same temperature for 1 h
  3. stirringThen the reaction mixture was stirred at room temperature for 20 h
  4. customAfter removal of the molecular sieves through celite pad
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. dissolutionThe crude mass was dissolved in ethyl acetate (250 mL)
  7. washorganic part was washed with saturated solution of NaHCO3 (100 mL)
  8. dry with materialdried over Na2SO4
  9. concentrationconcentrated under reduced pressure
  10. customto get crude which
  11. customwas purified by column chromatography
  12. washeluting with 8% EtOAc/hexane

出典と根拠

ORDレコード
ord-73a4d5a4f37b4385bc7a6705668fa062
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09150557B1

反応ノート

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