Hydrochloric Acid → (S)-[[1-(2-[[(1-amino-6-isoquinolinyl)carbonyl]amino]-1-oxopropyl)piperidin-4-yl]oxy]acetic acid hydrochloride

HRID 636930ノート

反応式

HRID 636930 の反応式
C([C@H:5]([O:9][CH:10]1[CH2:15][CH2:14][N:13]([C:16](=[O:33])[CH:17]([NH:19][C:20]([C:22]2[CH:23]=[C:24]3[C:29](=[CH:30][CH:31]=2)[C:28]([NH2:32])=[N:27][CH:26]=[CH:25]3)=[O:21])[CH3:18])[CH2:12][CH2:11]1)[C:6]([OH:8])=[O:7])(C)(C)C.[ClH:34]>O1CCOCC1>[ClH:34].[NH2:32][C:28]1[C:29]2[C:24](=[CH:23][C:22]([C:20]([NH:19][C@@H:17]([CH3:18])[C:16]([N:13]3[CH2:12][CH2:11][CH:10]([O:9][CH2:5][C:6]([OH:8])=[O:7])[CH2:15][CH2:14]3)=[O:33])=[O:21])=[CH:31][CH:30]=2)[CH:25]=[CH:26][N:27]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 86588687tert-butyl (S)-[[1-(2-[[(1-amino-6-isoquinolinyl)carbonyl]amino]-1-oxopropyl)piperidin-4-yl]oxy]acetic acid

生成物 1

HCID 69780722(S)-[[1-(2-[[(1-amino-6-isoquinolinyl)carbonyl]amino]-1-oxopropyl)piperidin-4-yl]oxy]acetic acid hydrochloride

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

To a solution of 594 mg of tert-butyl (S)-[[1-(2-[[(1-amino-6-isoquinolinyl)carbonyl]amino]-1-oxopropyl)piperidin-4-yl]oxy]acetic acid in 8 mL of dioxane was added 3 mL 36% hydrochloric acid and stirred at room temperature for two hours. The solution was concentrated and trituration of the residue with diethyl ether yielded 560 mg of the title compound. HPLC Supelcosil LC-18-DB column using a gradient elution system of 20% A/80% B to 20% A/20% B/60% C over 40 min at a flow of 0.25 ml/min (A: 0.5M phosphate buffer pH 2.1, B: water, C acetonitril/water 3/2 v/v). Rt=22.4 min.

後処理

  1. concentrationThe solution was concentrated

出典と根拠

ORDレコード
ord-1aafb86d2ecc484bb0f71b66cbcdf65d
出典データセット
uspto-grants-2001_02
特許番号
US06194409B1

反応ノート

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