Sodium hydride → HCID 86662320, 화합물

HRID 449643노트

반응식

HRID 449643 반응식
[CH3:1][N:2]([CH3:8])[CH2:3][C:4]([CH3:7])([OH:6])[CH3:5].[Br:9][C:10]1[N:11]=[N:12][C:13](Br)=[CH:14][CH:15]=1.[H-].[Na+]>C1COCC1>[Br:9][C:10]1[N:11]=[N:12][C:13]([O:6][C:4]([CH3:7])([CH3:5])[CH2:3][N:2]([CH3:8])[CH3:1])=[CH:14][CH:15]=1

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 2488523,6-DibromopyridazineHCID 97937381-(Dimethylamino)-2-methylpropan-2-ol

생성물 1

HCID 86662320HCID 86662320, 화합물수율 65.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
0 °C

실험 절차

In a 100 mL round bottom flask was added 1-(dimethylamino)-2-methylpropan-2-ol (1.48 g, 12.6 mmol, Eq: 1.5), THF and 3,6-dibromopyridazine (2 g, 8.41 mmol, Eq: 1.00). The flask was cooled to 0° C. followed by addition of NaH (572 mg, 14.3 mmol, Eq: 1.7) in one portion. The turbid reaction mixture was allowed to warm to room temperature and was stirred at room temperature overnight. The resultant black reaction mixture was absorbed onto silica gel and purified by LC chromatography eluting with 0-5% MeOH in 1/1 EtOAc/Hex to afford 1.5 g (65%) of the title compound.

후처리

  1. customThe turbid reaction mixture
  2. temperatureto warm to room temperature
  3. customThe resultant black reaction mixture
  4. customwas absorbed onto silica gel
  5. custompurified by LC chromatography
  6. washeluting with 0-5% MeOH in 1/1 EtOAc/Hex

출처 및 근거

ORD 기록
ord-40e996f4ac5b45199b6b38b6571d5db8
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08481540B2

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