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Bromine → HCID 178490292, 화합물

HRID 1244760
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HRID 1244760 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:11][CH2:12][NH:13][C:14]2[N:22]=[C:21]3[C:17]([N:18]=[CH:19][NH:20]3)=[C:16]([N:23]3[CH2:28][CH2:27][O:26][CH2:25][CH2:24]3)[N:15]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[Br:29]Br>O1CCOCC1.O>[Br:29][C:19]1[NH:20][C:21]2[C:17]([N:18]=1)=[C:16]([N:23]1[CH2:28][CH2:27][O:26][CH2:25][CH2:24]1)[N:15]=[C:14]([NH:13][CH2:12][CH2:11][C:5]1[CH:6]=[CH:7][C:8]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:4]=1)[N:22]=2
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참가 물질

5

반응물 2

HCID 24408BromineHCID 178490293HCID 178490293, 화합물

생성물 1

HCID 178490292HCID 178490292, 화합물수율 75.5%

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매2회

실험 절차

To a solution of [2-(3,4-dimethoxy-phenyl)-ethyl]-(6-morpholin-4-yl-9H-purin-2-yl) amine (1.16 g, 3 mmol) in dioxane (75 mL) was added bromine (0.180 mL, 3.3 mmol) in dioxane (5 mL) dropwise over a period of 1 hour. The mixture was stirred at room temperature for additional 4 hours and diluted with water (25 mL) and extracted with EtOAc. The organic phase was washed with brine, water, dried over Na2SO4. The solvent was evaporated in vacuo and solid was washed with methanol to give (8-bromo-6-morpholin-4-yl-9H-purin-2-yl)-[2-(3,4-dimethoxy-phenyl)-ethyl]-amine as a white solid (1.05 g, 75% yield).

후처리

  1. extractionextracted with EtOAc
  2. washThe organic phase was washed with brine, water
  3. dry with materialdried over Na2SO4
  4. customThe solvent was evaporated in vacuo and solid
  5. washwas washed with methanol

출처 및 근거

ORD 기록
ord-05e58af8ab144e3589ff161cc189ac98
출처 데이터셋
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07122665B2

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