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Methylamine → HCID 11617294, 화합물

HRID 659990
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HRID 659990 반응식
[Cl:1][CH2:2][C:3]1[N:12]([CH2:13][CH2:14][CH3:15])[C:11](=[O:16])[C:10]2[C:5](=[C:6]([OH:19])[C:7]([Cl:18])=[CH:8][C:9]=2[Cl:17])[N:4]=1.[CH3:20][NH2:21]>C1COCC1.C(O)C>[ClH:1].[Cl:17][C:9]1[CH:8]=[C:7]([Cl:18])[C:6]([OH:19])=[C:5]2[C:10]=1[C:11](=[O:16])[N:12]([CH2:13][CH2:14][CH3:15])[C:3]([CH2:2][NH:21][CH3:20])=[N:4]2
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참가 물질

5

반응물 2

HCID 6329MethylamineHCID 45118229HCID 45118229, 화합물

생성물 1

HCID 11617294HCID 11617294, 화합물수율 50%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 2-chloromethyl-5,7-dichloro-8-hydroxy-3-n-propyl-3H-quinazolin-4-one (285 mg, 0.886 mmol) in anhydrous THF (1.3 mL) was added a solution of methylamine in ethanol (7.5 mL of a 8.0M solution, 60 mmol) dropwise under an argon atmosphere. The mixture was stirred at room temperature for 18 h, then concentrated, and to the resulting residue was added 2M HCl (5 mL). The mixture was evaporated and more 2M HCl (5 mL) was added. The residue was evaporated and the procedure repeated two more times. The mixture was triturated with dichloromethane and dried in vacuo to yield 5,7-dichloro-8-hydroxy-2-methylaminomethyl-3-n-propyl-3H-quinazolin-4-one hydrochloride (4-9A) as a yellow solid (157 mg, 50%)(Table 6).

후처리

  1. concentrationconcentrated
  2. additionto the resulting residue was added 2M HCl (5 mL)
  3. customThe mixture was evaporated
  4. additionmore 2M HCl (5 mL) was added
  5. customThe residue was evaporated
  6. customThe mixture was triturated with dichloromethane
  7. customdried in vacuo

출처 및 근거

ORD 기록
ord-d5bafb3727184923b0f5610daa4ad0ce
출처 데이터셋
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08084459B2

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