Bromine → N-(4-bromo-2-methylthiazol-5-yl)acetamide

HRID 1051426노트

반응식

HRID 1051426 반응식
[CH3:1][C:2]1[S:3][C:4]([NH:7][C:8](=[O:10])[CH3:9])=[CH:5][N:6]=1.[Br:11]Br>C(Cl)(Cl)Cl.OS([O-])=O.[Na+]>[Br:11][C:5]1[N:6]=[C:2]([CH3:1])[S:3][C:4]=1[NH:7][C:8](=[O:10])[CH3:9]

참가 물질

5

반응물 2

HCID 24408BromineHCID 73554716N-(2-Methylthiazol-5-yl)acetamide

생성물 1

HCID 86715559N-(4-bromo-2-methylthiazol-5-yl)acetamide수율 67%

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 23665763Sodium Bisulfite용매

실험 절차

To a solution of N-(2-methylthiazol-5-yl)acetamide (0.4 g, 2.6 mmol) in CHCl3 (30 mL) was added Br2 (0.15 mL, 2.8 mmol), then the solution was stirred at room temperature for 12 h to give a brown solution. The reaction mixture was diluted with saturated NaHSO3 solution. The aqueous layer was extracted with DCM (3×30 mL). The combined organic layers were dried with Na2SO4, filtered and concentrated to afford a yellow solid. The resulting mixture was deposited onto silica gel and loaded onto a silica gel column and eluted with PE/EA(1:1) to give the title compound (400 mg, yield 67%).

후처리

  1. customto give a brown solution
  2. extractionThe aqueous layer was extracted with DCM (3×30 mL)
  3. dry with materialThe combined organic layers were dried with Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customto afford a yellow solid
  7. washeluted with PE/EA(1:1)

출처 및 근거

ORD 기록
ord-432fd5a06d8249868afbdf458b1a3e7c
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09388180B2

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