Isopropanol → 2-(2-Amino-6-phenoxy-4h-pyrido[3,4-d]pyrimidin-3-yl)-3,n-dimethyl-n-phenethyl-butyramide hydrochloride salt

HRID 491918ノート

反応式

HRID 491918 の反応式
[NH2:1][C:2]1[C:3]([CH2:15][NH:16][CH:17]([CH:30]([CH3:32])[CH3:31])[C:18]([N:20]([CH3:29])[CH2:21][CH2:22][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)=[O:19])=[CH:4][C:5]([O:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[N:6][CH:7]=1.C(O)(C)C.[N:37]#[C:38]Br.[Cl:40]CCl>>[ClH:40].[NH2:37][C:38]1[N:16]([CH:17]([CH:30]([CH3:32])[CH3:31])[C:18]([N:20]([CH3:29])[CH2:21][CH2:22][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)=[O:19])[CH2:15][C:3]2[CH:4]=[C:5]([O:8][C:9]3[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=3)[N:6]=[CH:7][C:2]=2[N:1]=1

参加物

5

反応物 4

HCID 3776IsopropanolHCID 6344DichloromethaneHCID 10476Cyanogen BromideHCID 670236882-[(5-Amino-2-phenoxy-pyridin-4-ylmethyl)-amino]-3,N-dimethyl-N-phenethyl-butyramide

生成物 1

HCID 670237612-(2-Amino-6-phenoxy-4h-pyrido[3,4-d]pyrimidin-3-yl)-3,n-dimethyl-n-phenethyl-butyramide hydrochloride salt

実験手順

A solution of 2-[(5-amino-2-phenoxy-pyridin-4-ylmethyl)-amino]-3,N-dimethyl-N-phenethyl-butyramide (1.69 g, 3.9 mmol) and isopropyl alcohol (10 mL) was added cyanogen bromide in dichloromethane (1.3 mL, [3M]) and the resulting mixture was stirred at room temperature for 16 hours. The solvent was evaporated to yield a brown solid. The brown solid was purified by reverse phase chromatography. The solvent was evaporated from the desired fractions, and the solute was treated with 1N HCl to yield the title compound as a solid, as its corresponding hydrochloride salt.

後処理

  1. customThe solvent was evaporated
  2. customto yield a brown solid
  3. customThe brown solid was purified by reverse phase chromatography
  4. customThe solvent was evaporated from the desired fractions
  5. additionthe solute was treated with 1N HCl

出典と根拠

ORDレコード
ord-fe43abca38544525a56879bb21a7a7be
出典データセット
uspto-grants-2009_05
特許番号
US07531545B2

反応ノート

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