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Toluene → HCID 57691362, 화합물

HRID 40225
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HRID 40225 반응식
[C:1]1([C:7]2[CH:8]=[N:9][C:10]3[N:11]([C:13]([CH2:16]O)=[N:14][N:15]=3)[N:12]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl.C(N1C=C(C2C=CC3N(C(CN)=[N:34][N:35]=3)N=2)C=N1)(C)C.C1CCN2C(=[N:42]CCC2)CC1.C1(C)C=CC=CC=1>>[N:42]([CH2:16][C:13]1[N:11]2[N:12]=[C:7]([C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)[CH:8]=[N:9][C:10]2=[N:15][N:14]=1)=[N+:34]=[N-:35]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 1140TolueneHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 675025246-Phenyl-1,2,4-triazolo[4,3-b][1,2,4]triazine-3-methanolHCID 67503644(6-(1-isopropyl-1H-pyrazol-4-yl)-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)methanamine hydrochloride

생성물 1

HCID 57691362HCID 57691362, 화합물

실험 절차

A 16 mm test tube was charged with (6-phenyl-[1,2,4]triazolo[4,3-b][1,2,4]triazin-3-yl)methanol (0.500 g, 2.20 mmol), Reactant 2 (0.951 ml, 4.40 mmol), DBU (0.663 ml, 4.40 mmol), and toluene (8.16 ml, 77.0 mmol), flushed with argon, sealed, then stirred at room temperature for 3 hours. The dark maroon mixture was concentrated and the resulting dark purple/black oil was purified by column chromatography using a gradient of 3-5% MeOH/DCM over 20 minutes. 3-(azidomethyl)-6-phenyl-[1,2,4]triazolo[4,3-b][1,2,4]triazine was isolated as a brown solid.

후처리

  1. customflushed with argon
  2. customsealed
  3. concentrationThe dark maroon mixture was concentrated
  4. customthe resulting dark purple/black oil was purified by column chromatography
  5. customover 20 minutes

출처 및 근거

ORD 기록
ord-8738196341d44914b3c9bc3aa591c901
출처 데이터셋
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08524900B2

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