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Diisopropylethylamine → Tert-Butyl 4-(3-(Tert-Butyldisulfanyl)-2-(Isobutoxycarbonylamino)Propanamido)Piperidine-1-Carboxylate

HRID 923720
ノート
印刷プレビュー

反応式

HRID 923720 の反応式
[C:1]([S:5][S:6][CH2:7][CH:8]([NH:12][C:13]([O:15][CH2:16][CH:17]([CH3:19])[CH3:18])=[O:14])[C:9]([OH:11])=O)([CH3:4])([CH3:3])[CH3:2].CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C.[C:53]([N:60]1[CH2:65][CH2:64][CH:63]([NH2:66])[CH2:62][CH2:61]1)([O:55][C:56]([CH3:59])([CH3:58])[CH3:57])=[O:54]>CN(C=O)C>[C:1]([S:5][S:6][CH2:7][CH:8]([NH:12][C:13]([O:15][CH2:16][CH:17]([CH3:19])[CH3:18])=[O:14])[C:9]([NH:66][CH:63]1[CH2:62][CH2:61][N:60]([C:53]([O:55][C:56]([CH3:59])([CH3:58])[CH3:57])=[O:54])[CH2:65][CH2:64]1)=[O:11])([CH3:2])([CH3:3])[CH3:4]
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 4

HCID 81531DiisopropylethylamineHCID 12682914-Amino-1-Boc-piperidineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 871033123-(Tert-Butyldisulfanyl)-2-(Isobutoxycarbonylamino)Propanoic Acid

生成物 1

HCID 87107224Tert-Butyl 4-(3-(Tert-Butyldisulfanyl)-2-(Isobutoxycarbonylamino)Propanamido)Piperidine-1-Carboxylate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To the acid from Example 59 (6.98 g, 22.6 mmol) in DMF (50 ml was added HATU (8.58 g, 22.6 mmol). After 30 min, Hunig base (4.71 ml, 27.1 mmol) and 1-Boc-4-amino piperidine (5.43 g, 27.1 mmol) were added to the mixture. The reaction was continued stirring at RT for another 3 h. DMF was removed at high vacuum, the crude residue was dissolved in EtAc (300 ml), washed with H2O (50 ml×3). The title compound was obtained after ISCO purification (5% MeOH/DCM).

後処理

  1. customDMF was removed at high vacuum
  2. dissolutionthe crude residue was dissolved in EtAc (300 ml)
  3. washwashed with H2O (50 ml×3)

出典と根拠

ORDレコード
ord-42028ecd482a4a6fa8304391e0a2b61f
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09278987B2

反応ノート

読み込み中…

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