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

HRID 2304250노트

반응식

HRID 2304250 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  1. concentrationThe solution was concentrated

출처 및 근거

ORD 기록
ord-fa8662200606450597046b1c36a10d82
출처 데이터셋
uspto-grants-2002_08
특허 번호
US06432955B1

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