Acetic Acid → Methyl 2-(3-((4-(2-amino-4-methyl-6-(pentylamino)pyrimidin-5-yl)butylamino)methyl)phenyl)acetate

HRID 1617134ノート

反応式

HRID 1617134 の反応式
[NH2:1][CH2:2][CH2:3][CH2:4][CH2:5][C:6]1[C:7]([NH:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19])=[N:8][C:9]([NH2:13])=[N:10][C:11]=1[CH3:12].[CH:20]([C:22]1[CH:23]=[C:24]([CH2:28][C:29]([O:31][CH3:32])=[O:30])[CH:25]=[CH:26][CH:27]=1)=O.C(O)(=O)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>C1COCC1>[NH2:13][C:9]1[N:10]=[C:11]([CH3:12])[C:6]([CH2:5][CH2:4][CH2:3][CH2:2][NH:1][CH2:20][C:22]2[CH:23]=[C:24]([CH2:28][C:29]([O:31][CH3:32])=[O:30])[CH:25]=[CH:26][CH:27]=2)=[C:7]([NH:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19])[N:8]=1

参加物

6

反応物 4

HCID 176Acetic AcidHCID 5049666Sodium triacetoxyborohydrideHCID 11819590Methyl 2-(3-formylphenyl)acetateHCID 684176515-(4-Aminobutyl)-6-methyl-N4-pentylpyrimidine-2,4-diamine

生成物 1

HCID 42612993Methyl 2-(3-((4-(2-amino-4-methyl-6-(pentylamino)pyrimidin-5-yl)butylamino)methyl)phenyl)acetate収率 6.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To the product of step (ii) (0.06 g), methyl 2-(3-formylphenyl)acetate (0.0403 g) and acetic acid (0.0136 g) in THF (10 mL) was added sodium triacetoxyborohydride (0.1102 g). The reaction mixture was stirred for 72 h, the solvents were evaporated and the residue dissolved in MeOH, acidified and purified via SCX resin, then RPHPLC to give the title compound 6 mg.

後処理

  1. customthe solvents were evaporated
  2. dissolutionthe residue dissolved in MeOH
  3. custompurified via SCX resin

出典と根拠

ORDレコード
ord-407031267df042b6af45a046affb603f
出典データセット
uspto-grants-2014_07
特許番号
US08765939B2

反応ノート

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