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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Hydrochloric Acid → 6-Methyl-2,4,8,22-tetraazatetracyclo[14.3.1.1(3,7).1(9,13)]docosa-1(20),3(22),4,6,9(21),10,12,16,18-nonaen-12-amine

HRID 541903
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HRID 541903 반응식
Cl.Cl.Cl.[NH2:4][C:5]1[CH:6]=[C:7]([CH2:11][CH2:12][C:13]2[CH:18]=[C:17]([NH:19][C:20]3[C:25]([CH3:26])=[CH:24][N:23]=[C:22](Cl)[N:21]=3)[CH:16]=[CH:15][C:14]=2[NH2:28])[CH:8]=[CH:9][CH:10]=1.Cl.O.[OH-].[Na+]>COCCO.O1CCOCC1>[CH3:26][C:25]1[CH:24]=[N:23][C:22]2[NH:4][C:5]3[CH:10]=[CH:9][CH:8]=[C:7]([CH:6]=3)[CH2:11][CH2:12][C:13]3[CH:18]=[C:17]([NH:19][C:20]=1[N:21]=2)[CH:16]=[CH:15][C:14]=3[NH2:28]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 14798Sodium HydroxideHCID 866362872-[2-(3-Aminophenyl)ethyl]-N(4)-(2-chloro-5-methylpyrimidin-4-yl)benzene-1,4-diamine Trihydrochloride

생성물 1

HCID 579623606-Methyl-2,4,8,22-tetraazatetracyclo[14.3.1.1(3,7).1(9,13)]docosa-1(20),3(22),4,6,9(21),10,12,16,18-nonaen-12-amine수율 48%

시약·촉매·용매 2

HCID 80192-Methoxyethanol용매HCID 312751,4-Dioxane용매

실험 절차

To a solution of 2-[2-(3-aminophenyl)ethyl]-N(4)-(2-chloro-5-methylpyrimidin-4-yl)benzene-1,4-diamine trihydrochloride (0.16 g, 0.45 mmol) in 2-methoxyethanol (2 mL) was added 4.0 M of hydrogen chloride in 1,4-dioxane (110 μL). The resultant mixture was heated at 150° C. in the microwave for 15 min. After cooling, water and NaOH (12 N) were added to neutralize the mixture to pH=7. The aqueous layer was extracted with EtOAc four times. The combined organic layers were dried, filtered and concentrated. The residue was purified by silica gel column chromatography to give the desired product as an off-white powder (60 mg, 48%). LCMS for C19H20N5 (M+H)+: m/z=318.2.

후처리

  1. temperatureAfter cooling
  2. extractionThe aqueous layer was extracted with EtOAc four times
  3. customThe combined organic layers were dried
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-f09dd5814fb240b18709d1864b890720
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08871753B2

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