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Ethyl bromoacetate → HCID 56598352, 화합물

HRID 535452
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HRID 535452 반응식
Br[CH2:2][C:3]([O:5][CH2:6][CH3:7])=[O:4].C(N(CC)CC)C.[OH:15][N:16]1[C:25](=[O:26])[C:24]2[C:19](=[CH:20][CH:21]=[C:22]([C:27]([C:29]3[N:37]4[C:32]([CH:33]=[CH:34][CH:35]=[CH:36]4)=[C:31]([O:38][CH3:39])[C:30]=3[CH3:40])=[O:28])[CH:23]=2)[NH:18][C:17]1=[O:41]>C(O)C>[CH2:6]([O:5][C:3](=[O:4])[CH2:2][O:15][N:16]1[C:25](=[O:26])[C:24]2[C:19](=[CH:20][CH:21]=[C:22]([C:27]([C:29]3[N:37]4[C:32]([CH:33]=[CH:34][CH:35]=[CH:36]4)=[C:31]([O:38][CH3:39])[C:30]=3[CH3:40])=[O:28])[CH:23]=2)[NH:18][C:17]1=[O:41])[CH3:7]
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참가 물질

5

반응물 3

HCID 7748Ethyl bromoacetate2회HCID 8471Triethylamine2회HCID 66653429HCID 66653429, 화합물

생성물 1

HCID 56598352HCID 56598352, 화합물수율 48.6%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

0.11 ml (0.99 mmol) of ethyl bromoacetate and then 0.14 ml (0.99 mmol) of triethylamine are added, at ambient temperature under an inert atmosphere, to 0.36 g (0.99 mmol) of 3-hydroxy-6-[(1-methoxy-2-methylindolizin-3-yl)carbonyl]quinazoline-2,4(1H,3H)-dione in 12.5 ml of ethanol. The reaction medium is stirred for 18 hours and then 0.14 ml (0.99 mmol) of triethylamine and 0.11 ml (0.99 mmol) of ethyl bromoacetate are added. After stirring for 18 hours at ambient temperature, the reaction medium is concentrated under reduced pressure. The residue obtained is purified by silica gel column chromatography, elution being carried out with a dichloromethane/methanol mixture. 217 mg of a yellow powder are obtained.

후처리

  1. stirringAfter stirring for 18 hours at ambient temperature
  2. concentrationthe reaction medium is concentrated under reduced pressure
  3. customThe residue obtained
  4. customis purified by silica gel column chromatography, elution

출처 및 근거

ORD 기록
ord-83fbb5dc57cb4ca481acbf8cb33185a1
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08859544B2

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