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

HRID 10530ノート

反応式

HRID 10530 の反応式
[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

参加物

3

反応物 2

HCID 21893726Hydrochloride methanolHCID 21979971HCID 21979971、化合物

生成物 1

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-daedd6bee30f484fb7b742c746a69337
出典データセット
uspto-grants-2006_08
特許番号
US07094789B2

反応ノート

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