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Water → HCID 22007304, 화합물

HRID 323877
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HRID 323877 반응식
C(=O)([O-])[O-].[K+].[K+].[CH3:7][N:8]1[C:16]2[N:15]=[CH:14][N:13]([C:17]([C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=3)([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)[C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[C:12]=2[C:11](=[O:36])[NH:10][C:9]1=[O:37].[Cl:38][C:39]1[CH:49]=[CH:48][C:42]([CH2:43][O:44][CH2:45][CH2:46]Cl)=[CH:41][CH:40]=1.O>CN1CCCC1=O>[Cl:38][C:39]1[CH:40]=[CH:41][C:42]([CH2:43][O:44][CH2:45][CH2:46][N:10]2[C:11](=[O:36])[C:12]3[N:13]([C:17]([C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=4)([C:30]4[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=4)[C:18]4[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=4)[CH:14]=[N:15][C:16]=3[N:8]([CH3:7])[C:9]2=[O:37])=[CH:48][CH:49]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 2235351-Chloro-4-[(2-chloroethoxy)methyl]benzene2회HCID 22007310HCID 22007310, 화합물

생성물 1

HCID 22007304HCID 22007304, 화합물

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone
용매

실험 절차

1.3 g (9.44 mmol) of potassium carbonate were added at 60° C. to a solution of 2.4 g (5.9 mmol) of 3-methyl-7-tritylxanthine (prepared according to Example 17a) in 50 ml of N-methylpyrrolidone and the mixture was stirred at this temperature for one hour. 1.57 g (7.67 mmol) of 2-(4-chlorobenzyloxy)ethyl chloride were then added dropwise and the mixture was stirred at 80° C. for one hour. A further 1.0 g (4.9 mmol) of 2-(4-chlorobenzyloxy)ethyl chloride was then added and the mixture was stirred again for one hour. 50 ml of water were then added, the mixture was extracted three times using 60 ml of methyl tert-butyl ether each time, and the combined organic phases were washed twice with 30 ml of water each time, dried using magnesium sulfate and concentrated under reduced pressure. The crude product was purified by flash chromatography on a silica gel column, heptane/ethyl acetate (3/2).

후처리

  1. stirringthe mixture was stirred at 80° C. for one hour
  2. stirringthe mixture was stirred again for one hour
  3. extractionthe mixture was extracted three times
  4. washthe combined organic phases were washed twice with 30 ml of water each time
  5. customdried
  6. concentrationconcentrated under reduced pressure
  7. customThe crude product was purified by flash chromatography on a silica gel column, heptane/ethyl acetate (3/2)

출처 및 근거

ORD 기록
ord-12e1351a79ff47619b58315c6d38dbef
출처 데이터셋
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06214992B1

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