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[4-({2-[(3,5-Diamino-6-chloro-pyrazine-2-carbonyl)-amino]-ethyl}-methyl-amino)-butyl]-carbamic acid tert-butyl ester → 3,5-Diamino-6-chloro-pyrazine-2-carboxylic acid {2-[(4-amino-butyl)-methyl-amino]-ethyl}-amide

HRID 882920
ノート
印刷プレビュー

反応式

HRID 882920 の反応式
C(OC(=O)[NH:7][CH2:8][CH2:9][CH2:10][CH2:11][N:12]([CH2:14][CH2:15][NH:16][C:17]([C:19]1[C:24]([NH2:25])=[N:23][C:22]([NH2:26])=[C:21]([Cl:27])[N:20]=1)=[O:18])[CH3:13])(C)(C)C>C(Cl)Cl.C(O)(C(F)(F)F)=O>[NH2:7][CH2:8][CH2:9][CH2:10][CH2:11][N:12]([CH3:13])[CH2:14][CH2:15][NH:16][C:17]([C:19]1[C:24]([NH2:25])=[N:23][C:22]([NH2:26])=[C:21]([Cl:27])[N:20]=1)=[O:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 86656659[4-({2-[(3,5-Diamino-6-chloro-pyrazine-2-carbonyl)-amino]-ethyl}-methyl-amino)-butyl]-carbamic acid tert-butyl ester

生成物 1

HCID 866566603,5-Diamino-6-chloro-pyrazine-2-carboxylic acid {2-[(4-amino-butyl)-methyl-amino]-ethyl}-amide

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 6422Trifluoroacetic acid溶媒

実験手順

[4-({2-[(3,5-Diamino-6-chloro-pyrazine-2-carbonyl)-amino]-ethyl}-methyl-amino)-butyl]-carbamic acid tert-butyl ester (0.54 g, 2.2 mmol) in DCM (10 mL) and TFA (2 mL) is stirred at RT for 1 h. The solvent is removed in vacuo and the resulting oil is dissolved in saturated aqueous sodium carbonate solution. The mixture is concentrated in vacuo and the residue is dissolved in MeOH and filtered to remove the sodium carbonate. The filtrate is concentrated in vacuo to afford the title compound. [M+H]+ 316

後処理

  1. customThe solvent is removed in vacuo
  2. dissolutionthe resulting oil is dissolved in saturated aqueous sodium carbonate solution
  3. concentrationThe mixture is concentrated in vacuo
  4. dissolutionthe residue is dissolved in MeOH
  5. filtrationfiltered
  6. customto remove the sodium carbonate
  7. concentrationThe filtrate is concentrated in vacuo

出典と根拠

ORDレコード
ord-f1d63dc399aa439f98825655c603913a
出典データセット
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08236808B2

反応ノート

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