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Diisopropylethylamine → (S)-3-(tert-butyldiphenylsilyloxy)-N1-(1-adamantylmethyl)propane-1,2-diamine

HRID 75159
ノート
印刷プレビュー

反応式

HRID 75159 の反応式
Cl.[NH2:2][C@@H:3]([CH2:6][NH:7][CH2:8][C:9]12[CH2:18][CH:13]3[CH2:14][CH:15]([CH2:17][CH:11]([CH2:12]3)[CH2:10]1)[CH2:16]2)[CH2:4][OH:5].CCN(C(C)C)C(C)C.[CH3:28][C:29]([Si:32](Cl)([C:39]1[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=1)[C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1)([CH3:31])[CH3:30]>C(Cl)Cl.CN(C1C=CN=CC=1)C>[Si:32]([O:5][CH2:4][C@@H:3]([NH2:2])[CH2:6][NH:7][CH2:8][C:9]12[CH2:18][CH:13]3[CH2:12][CH:11]([CH2:17][CH:15]([CH2:14]3)[CH2:16]1)[CH2:10]2)([C:29]([CH3:31])([CH3:30])[CH3:28])([C:39]1[CH:40]=[CH:41][CH:42]=[CH:43][CH:44]=1)[C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 81531DiisopropylethylamineHCID 94078tert-ButyldiphenylchlorosilaneHCID 68477778HCID 68477778、化合物

生成物 1

HCID 68474186(S)-3-(tert-butyldiphenylsilyloxy)-N1-(1-adamantylmethyl)propane-1,2-diamine収率 34.2%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒
HCID 6344
Dichloromethane
溶媒

実験手順

To a solution of (S)-2-amino-3-((1-adamantylmethyl)amino)propan-1-ol HCl salt (1.2 g, 3.8 mmol) in anhydrous CH2Cl2 (20 mL) were added DIEA (1.9 g, 15.2 mmol), DMAP (2.3 mg, 0.02 mmol) and TBDPSCl (1.2 g, 4.2 mmol) at 0° C. The mixture was stirred at rt for 2 h. The reaction solution was extracted with CH2Cl2 (100 mL) and water (20 mL). The organic layer was washed with brine (20 mL), dried over MgSO4, and concentrated to give the crude product, which was purified by preparative TLC (PE:EtOAc 10/1) to afford (S)-3-(tert-butyldiphenylsilyloxy)-N1-(1-adamantylmethyl)propane-1,2-diamine (620 mg, 29%) 1H NMR: (CDCl3, 400 MHz): δ=1.05 (s, 9H), 1.54 (s, 6H), 1.62-1.73 (m, 6H), 1.98 (s, 3H), 2.32 (d, 1H), 2.45 (d, 1H), 2.56 (d, 1H), 2.85 (d, 1H), 3.15 (m, 4H), 3.65 (m, 2H), 7.4 (m, 6H), 7.62 (m, 4H).

後処理

  1. extractionThe reaction solution was extracted with CH2Cl2 (100 mL) and water (20 mL)
  2. washThe organic layer was washed with brine (20 mL)
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated
  5. customto give the crude product, which
  6. customwas purified by preparative TLC (PE:EtOAc 10/1)

出典と根拠

ORDレコード
ord-c3e7ace0c19f4e1d9e9d57f0aadba26a
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08835426B2

反応ノート

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