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

HRID 491918노트

반응식

HRID 491918 반응식
[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

참가 물질

5

반응물 4

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

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fe43abca38544525a56879bb21a7a7be
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07531545B2

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