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Methanol → Methyl 4-(3-amino-6-(4-(hydroxymethyl)cyclohexyl)pyrazin-2-yl)-2-fluorobenzoate

HRID 596116
ノート
印刷プレビュー

反応式

HRID 596116 の反応式
[NH2:1][C:2]1[C:3]([C:23]2[CH:32]=[CH:31][C:26]([C:27]([O:29][CH3:30])=[O:28])=[C:25]([F:33])[CH:24]=2)=[N:4][C:5]([C:8]2[CH2:13][CH2:12][CH:11]([CH2:14][O:15]CC3C=CC=CC=3)[CH2:10][CH:9]=2)=[CH:6][N:7]=1.CO>C1COCC1.[Pd]>[NH2:1][C:2]1[C:3]([C:23]2[CH:32]=[CH:31][C:26]([C:27]([O:29][CH3:30])=[O:28])=[C:25]([F:33])[CH:24]=2)=[N:4][C:5]([CH:8]2[CH2:13][CH2:12][CH:11]([CH2:14][OH:15])[CH2:10][CH2:9]2)=[CH:6][N:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 887MethanolHCID 118046409Methyl 4-(3-amino-6-(4-((benzyloxy)methyl)cyclohex-1-en-1-yl)pyrazin-2-yl)-2-fluorobenzoate

生成物 1

HCID 118045488Methyl 4-(3-amino-6-(4-(hydroxymethyl)cyclohexyl)pyrazin-2-yl)-2-fluorobenzoate収率 70.5%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8028Tetrahydrofuran溶媒

実験手順

Methyl 4-(3-amino-6-(4-((benzyloxy)methyl)cyclohex-1-en-1-yl)pyrazin-2-yl)-2-fluorobenzoate (381 mg, 0.851 mmol) was dissolved in THF (5 mL) and then MeOH (15 mL) was added and then Pd—C (10% wet) (550 mg, 0.517 mmol) was added. The mixture was put under vacuum and purged with hydrogen and this cycle was repeated thrice and then finally under hydrogen overnight. After 14 h, LCMS indicated alkene saturation but only partial benzyl deprotection, and therefore another Pd—C (10% wet) (700 mg) was added and the mixture stirred at room temperature for another 5 h after which complete benzyl deprotection observed. The reaction mixture was filtered and concentrated in vacuo to afford 215.6 mg of the desired product as a mixture of diasteromers (cis/trans unspecified) (70%). LCMS (m/z): 360.2 (MH+), 0.71, 0.72 min.

後処理

  1. custompurged with hydrogen
  2. customfinally under hydrogen overnight
  3. additionanother Pd—C (10% wet) (700 mg) was added
  4. filtrationThe reaction mixture was filtered
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-369f7fa89e8d4a5689281315ecefb22e
出典データセット
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09242996B2

反応ノート

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