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1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → Tert-butyl[2-[n-[1-(1h-pyrrolo[2,3-c]pyridin-2-yl)ethyl]carbamoyl]ethyl]carbamate

HRID 1821878
ノート
印刷プレビュー

反応式

HRID 1821878 の反応式
Cl.Cl.[NH:3]1[C:7]2=[CH:8][N:9]=[CH:10][CH:11]=[C:6]2[CH:5]=[C:4]1[CH:12]([NH2:14])[CH3:13].[C:15]([NH:22][CH2:23][CH2:24][C:25](O)=[O:26])([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16].C(N(C(C)C)CC)(C)C.CCN=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1>C(Cl)Cl>[C:18]([O:17][C:15](=[O:16])[NH:22][CH2:23][CH2:24][C:25](=[O:26])[NH:14][CH:12]([C:4]1[NH:3][C:7]2=[CH:8][N:9]=[CH:10][CH:11]=[C:6]2[CH:5]=1)[CH3:13])([CH3:21])([CH3:19])[CH3:20]
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 5

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 76809N-((1,1-dimethylethoxy)carbonyl)-beta-alanineHCID 81531DiisopropylethylamineHCID 689820051h-Pyrrolo[2,3-c]pyridine-2-methanamine,a-methyl-,dihydrochloride

生成物 1

HCID 57893518
Tert-butyl[2-[n-[1-(1h-pyrrolo[2,3-c]pyridin-2-yl)ethyl]carbamoyl]ethyl]carbamate
収率 58%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 1-(1H-pyrrolo[2,3-c]pyridin-2-yl)ethylamine dihydrochloride (Example 75) (108 mg, 0.46 mmol), N-Boc-β-alanine (71 mg, 0.37 mmol), diisopropylethylamine (0.31 mL, 1.85 mmol), EDCI (78 mg, 0.41 mmol) and HOBt (catalytic amount) in methylene chloride (2.2 mL) was stirred at room temperature under a nitrogen atmosphere overnight (22 h). The reaction mixture was concentrated to dryness under reduced pressure. The residue was dissolved in CH2Cl2, washed with water and saturated NaHCO3, and dried over Na2SO4. Filtration and concentration provided tert-butyl[2-[N-[1-(1H-pyrrolo[2,3-c]pyridin-2-yl)ethyl]carbamoyl]ethyl]carbamate (70 mg, 58%) as a tan solid: 1H NMR (500 MHz, CD3OD) δ1.45 (9H, s), 1.63 (3H, d), 2.37-2.51 (2H, m), 3.30-3.42 (2H, m), 5.26-5.35 (1H, m), 6.43 (1H, s), 7.48-7.51 (1H, m), 7.99-8.05 (1H, m), 8.60 (1H, s); ESI MS m/z 333 [C17H24N4O3+H]+; HPLC (Method A) 95.9% (AUC), tR=14.39 min.

後処理

  1. concentrationThe reaction mixture was concentrated to dryness under reduced pressure
  2. dissolutionThe residue was dissolved in CH2Cl2
  3. washwashed with water and saturated NaHCO3
  4. dry with materialdried over Na2SO4
  5. filtrationFiltration and concentration

出典と根拠

ORDレコード
ord-2b37d128947c48f39067a318dac00bee
出典データセット
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07608627B2

反応ノート

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