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1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → (2S,5R)-tert-butyl 5-(N-(benzyloxy)-2-nitrophenylsulfonamido)-2-carbamoyl-piperidine-1-carboxylate

HRID 1406855
ノート
印刷プレビュー

反応式

HRID 1406855 の反応式
[NH4+].[Cl-].C1C=CC2N(O)N=[N:9]C=2C=1.CCN=C=NCCCN(C)C.CCN(C(C)C)C(C)C.[CH2:33]([O:40][N:41]([C@H:54]1[CH2:59][N:58]([C:60]([O:62][C:63]([CH3:66])([CH3:65])[CH3:64])=[O:61])[C@H:57]([C:67](O)=[O:68])[CH2:56][CH2:55]1)[S:42]([C:45]1[CH:50]=[CH:49][CH:48]=[CH:47][C:46]=1[N+:51]([O-:53])=[O:52])(=[O:44])=[O:43])[C:34]1[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1>CN(C=O)C.CCOC(C)=O>[CH2:33]([O:40][N:41]([C@H:54]1[CH2:59][N:58]([C:60]([O:62][C:63]([CH3:64])([CH3:65])[CH3:66])=[O:61])[C@H:57]([C:67](=[O:68])[NH2:9])[CH2:56][CH2:55]1)[S:42]([C:45]1[CH:50]=[CH:49][CH:48]=[CH:47][C:46]=1[N+:51]([O-:53])=[O:52])(=[O:44])=[O:43])[C:34]1[CH:35]=[CH:36][CH:37]=[CH:38][CH:39]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 25517Ammonium ChlorideHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 86700669(2S,5R)-5-(N-(benzyloxy)-2-nitrophenylsulfonamido)-1-(tert-butoxycarbonyl) piperidine-2-carboxylic acid

生成物 1

HCID 86700668
(2S,5R)-tert-butyl 5-(N-(benzyloxy)-2-nitrophenylsulfonamido)-2-carbamoyl-piperidine-1-carboxylate
収率 99%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

NH4Cl (1.39 g, 26.18 mmol), HOBt (3.53 g, 26.18 mmol), EDCI (5 g, 26.18 mmol), and DIPEA (8.44 g, 65.45 mmol) were added to a solution of (2S,5R)-5-(N-(benzyloxy)-2-nitrophenylsulfonamido)-1-(tert-butoxycarbonyl)piperidine-2-carboxylic acid (10 g, 18.7 mmol) in DMF (90 mL) The mixture was stirred at rt for 17 hrs, then, EtOAc (500 mL) was added. he mixture was washed with saturated sodium chloride (6×), dried over Na2SO4, and concentrated. The residue was washed with petroleum ether/EtOAc (95:5, 200 mL) to give (2S,5R)-tert-butyl 5-(N-(benzyloxy)-2-nitrophenylsulfonamido)-2-carbamoylpiperidine-1-carboxylate (9.9 g, 99%) which was used in the next step. ESI-MS (EI+, m/z): 535.0 [M+H]+.

後処理

  1. washhe mixture was washed with saturated sodium chloride (6×)
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated
  4. washThe residue was washed with petroleum ether/EtOAc (95:5, 200 mL)

出典と根拠

ORDレコード
ord-b052afa8ef66426dbfd55b1d77059f32
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08916709B2

反応ノート

読み込み中…

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