Hydrochloride methanol → 4-(Methylsulfanyl)-N-(piperidin-4-yl)isoquinolin-5-amine--hydrogen chloride (1/1)

HRID 10530노트

반응식

HRID 10530 반응식
[CH3:1][S:2][C:3]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][C:11]=2[NH:13][CH:14]2[CH2:19][CH2:18][N:17](C(OC(C)(C)C)=O)[CH2:16][CH2:15]2)[CH:6]=[N:5][CH:4]=1.[ClH:27].CO>>[ClH:27].[CH3:1][S:2][C:3]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][C:11]=2[NH:13][CH:14]2[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]2)[CH:6]=[N:5][CH:4]=1

참가 물질

3

반응물 2

HCID 21893726Hydrochloride methanolHCID 21979971HCID 21979971, 화합물

생성물 1

HCID 219797534-(Methylsulfanyl)-N-(piperidin-4-yl)isoquinolin-5-amine--hydrogen chloride (1/1)

실험 절차

According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 74 (214 mg) and 10% hydrogen chloride/methanol solution (5 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with methanol (2 ml) and diethyl ether (6 ml). The deposited precipitates were collected by filtration and washed with diethyl ether to obtain the title compound (154 mg) as brown powdery solid.

후처리

  1. custom(50° C., 2 hours)
  2. customthe solvent was evaporated under reduced pressure
  3. additionThe residue was added with methanol (2 ml) and diethyl ether (6 ml)
  4. customThe deposited precipitates
  5. filtrationwere collected by filtration
  6. washwashed with diethyl ether

출처 및 근거

ORD 기록
ord-daedd6bee30f484fb7b742c746a69337
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07094789B2

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