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1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → tert-butyl 2-(4-(5-methyl-3-oxo-1H-imidazo[1,5-c]imidazol-2(3H)-yl)-1-piperidinyl)-2-oxo-1-phenylethylcarbamate

HRID 1162303
ノート
印刷プレビュー

反応式

HRID 1162303 の反応式
[C:1]([N:8](C1C=CC=CC=1)[CH2:9][C:10]([OH:12])=O)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].[CH:19]1[CH:20]=[CH:21][C:22]2N(O)N=N[C:23]=2[CH:24]=1.CCN=C=NCCCN(C)C.Cl.Cl.[CH3:42][C:43]1[N:47]2[C:48](=[O:57])[N:49]([CH:51]3[CH2:56][CH2:55][NH:54][CH2:53][CH2:52]3)[CH2:50][C:46]2=[CH:45][N:44]=1>C(#N)C.C(N(CC)CC)C>[CH3:42][C:43]1[N:47]2[C:48](=[O:57])[N:49]([CH:51]3[CH2:56][CH2:55][N:54]([C:10](=[O:12])[CH:9]([NH:8][C:1](=[O:2])[O:3][C:4]([CH3:5])([CH3:6])[CH3:7])[C:23]4[CH:22]=[CH:21][CH:20]=[CH:19][CH:24]=4)[CH2:53][CH2:52]3)[CH2:50][C:46]2=[CH:45][N:44]=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 4

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 219056362-{[(Tert-butoxy)carbonyl](phenyl)amino}acetic acidHCID 230840945-methyl-2-(4-piperidinyl)-1,2-dihydro-3H-imidazo[1,5-c]imidazol-3-one dihydrochloride

生成物 1

HCID 23138346tert-butyl 2-(4-(5-methyl-3-oxo-1H-imidazo[1,5-c]imidazol-2(3H)-yl)-1-piperidinyl)-2-oxo-1-phenylethylcarbamate
収率 95.9%

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 8471Triethylamine溶媒

実験手順

Boc-phenylglycine (0.25 g) was dissolved in acetonitrile (10 ml). HOBt (0.23 g), WSC (0.29 g), triethylamine (0.2 ml) and 5-methyl-2-(4-piperidinyl)-1,2-dihydro-3H-imidazo[1,5-c]imidazol-3-one dihydrochloride (0.29 g) were added thereto, and mixed at room temperature for 15 hours. The solvent was distilled off under reduced pressure, and the residue was dissolved in ethyl acetate. The ethyl acetate solution was washed with a saturated aqueous sodium hydrogen carbonate solution and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain the title compound as a green oil (0.43 g, 95%).

後処理

  1. additionmixed at room temperature for 15 hours
  2. distillationThe solvent was distilled off under reduced pressure
  3. dissolutionthe residue was dissolved in ethyl acetate
  4. washThe ethyl acetate solution was washed with a saturated aqueous sodium hydrogen carbonate solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationThe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-4ea7662bdb634b32841c130ed1bdf057
出典データセット
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07820673B2

反応ノート

読み込み中…

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