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Water → trans-4-amino-1-tert-butoxycarbonyl(2S)-(tert-butyldiphenylsilyloxy)methylpyrrolidine

HRID 350514
ノート
印刷プレビュー

反応式

HRID 350514 の反応式
Br[C@@H:2]1[CH2:6][N:5]([C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])[C@H:4]([CH2:14][O:15][Si:16]([C:29]([CH3:32])([CH3:31])[CH3:30])([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH2:3]1.[N-:33]=[N+]=[N-].[Na+].O>CN(C=O)C.CCO.[Pd]>[NH2:33][C@H:2]1[CH2:6][N:5]([C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])[C@H:4]([CH2:14][O:15][Si:16]([C:29]([CH3:32])([CH3:31])[CH3:30])([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH2:3]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 962WaterHCID 33557Sodium AzideHCID 69334767cis-4-bromo-1-tert-butoxycarbonyl-(2S)-(tert-butyldiphenylsilyloxy)methylpyrrolidine

生成物 1

HCID 69332987trans-4-amino-1-tert-butoxycarbonyl(2S)-(tert-butyldiphenylsilyloxy)methylpyrrolidine収率 95%

試薬・触媒・溶媒 3

HCID 23938Palladium触媒
HCID 702
Ethanol
溶媒
HCID 6228Dimethylformamide溶媒

実験手順

To a stirred solution of cis-4-bromo-1-tert-butoxycarbonyl-(2S)-(tert-butyldiphenylsilyloxy) methylpyrrolidine (480 mg, 0.93 mmol) in DMF (5 ml) was added NaN3 (241 mg, 3.70 mmol) at room temperature. The reaction mixture was stirred at 70 for 3 days. Water was added thereto, and extracted with EtOAc. The extract was washed with water, then dried over Na2SO4, and concentrated in vacuo. The crude product was used to the subsequent reaction without further purification. The solution of the crude residue in EtOH (10 ml) was hydrogenated over 10% Pd—C under an atmospheric pressure at room temperature for 4 hr. The catalyst was filtered off, and the filtrate was concentrated in vacuo to give trans-4-amino-1tert-butoxycarbonyl-(2S)-(tert-butyldiphenylsilyloxy)methylpyrrolidine (400 mg, 95%) as a colorless oil. 1H-NMR (CDCl3) δ 1.06 (s, 9H), 1.32 and 1.45 (each s, total 9H), 2.20–2.35 (m, 1H), 3.05–3.18 (m, 1H), 3.55–4.05 (m, 6H), 7.35–7.41 (m, 6H), 7.61–7.69 (m, 4H).

後処理

  1. extractionextracted with EtOAc
  2. washThe extract was washed with water
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated in vacuo
  5. customThe crude product was used to the subsequent reaction without further purification
  6. filtrationThe catalyst was filtered off
  7. concentrationthe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-9035888213764b3ea0846d5050d64283
出典データセット
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07179819B2

反応ノート

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