Ethyl Bromide → HCID 24964732, 화합물

HRID 1161867노트

반응식

HRID 1161867 반응식
[CH:1]([NH:4][C:5](=[O:33])[CH2:6][N:7]1[C:16](=[O:17])[C:15]2[C:10](=[CH:11][CH:12]=[C:13]([N:18]3[CH2:24][CH2:23][CH2:22][NH:21][CH2:20][CH2:19]3)[CH:14]=2)[N:9]=[C:8]1[C:25]1[CH:30]=[CH:29][CH:28]=[C:27]([O:31][CH3:32])[CH:26]=1)([CH3:3])[CH3:2].[CH2:34](Br)[CH3:35].C([O-])([O-])=O.[K+].[K+]>C(#N)C>[CH2:34]([N:21]1[CH2:22][CH2:23][CH2:24][N:18]([C:13]2[CH:14]=[C:15]3[C:10](=[CH:11][CH:12]=2)[N:9]=[C:8]([C:25]2[CH:30]=[CH:29][CH:28]=[C:27]([O:31][CH3:32])[CH:26]=2)[N:7]([CH2:6][C:5]([NH:4][CH:1]([CH3:3])[CH3:2])=[O:33])[C:16]3=[O:17])[CH2:19][CH2:20]1)[CH3:35]

참가 물질

5

반응물 3

HCID 6332Ethyl BromideHCID 11430Potassium CarbonateHCID 59519020HCID 59519020, 화합물

생성물 1

HCID 24964732HCID 24964732, 화합물수율 10%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of N-isopropyl-2-[2-(3-methoxyphenyl)-4-oxo-6-perhydro-1,4-diazepin-1-yl-4H-quinazolin-3-yl]acetamide (EXAMPLE 2a) hydrochloride salt (50 mg, 0.103 mmol), ethyl bromide (22 mg, 0.21 mmol), and K2CO3 (43 mg, 0.31 mmol) in acetonitrile (5 mL) was heated to reflux for 24 h. The mixture was then cooled, filtered and concentrated in vacuo. The crude residue was purified by preparative HPLC to afford 2-[6-(4-ethylperhydro-1,4-diazepin-1-yl)-2-(3-methoxyphenyl)-4-oxo-4H-quinazolin-3-yl]-N-isopropylacetamide (EXAMPLE 4a) (5.1 mg, 0.010 mmol, 10%) as the hydrochloride salt.

후처리

  1. temperaturewas heated
  2. temperatureto reflux for 24 h
  3. temperatureThe mixture was then cooled
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe crude residue was purified by preparative HPLC

출처 및 근거

ORD 기록
ord-908b7fc54c1148d7aa284ce2398c0e40
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07820649B2

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