Bromine → HCID 57634025, 화합물

HRID 661063노트

반응식

HRID 661063 반응식
[CH3:1][N:2]([CH2:4][C:5]1[N:6]=[C:7]([NH:10][C:11](=[O:13])[CH3:12])[S:8][CH:9]=1)[CH3:3].[Br:14]Br>CC(O)=O>[Br:14][C:9]1[S:8][C:7]([NH:10][C:11](=[O:13])[CH3:12])=[N:6][C:5]=1[CH2:4][N:2]([CH3:1])[CH3:3]

참가 물질

4

반응물 2

HCID 24408BromineHCID 57634222N-[4-[(Dimethylamino)methyl]-2-thiazolyl]acetamide

생성물 1

HCID 57634025HCID 57634025, 화합물수율 65.4%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

To a solution of N-(4-((dimethylamino)methyl)thiazol-2-yl)acetamide (1.1 g, 5.5 mmol) in 10 mL AcOH was added Br2 (0.28 mL, 5.5 mmol) dropwise. The resulting mixture discolored instantly, and a precipitate appeared. The precipitate was filtered and washed with AcOH. The collected precipitate was neutralized with saturated sodium bicarbonate and extracted twice with 100 mL EtOAc. The organic layer was combined, washed once with brine, and dried over sodium sulfate. After removing the solvent, the product was obtained as a white solid (1.0 g, yield=65%). LCMS (API-ES) m/z (%) 278.0 (100%, M++H). 1H NMR (400 MHz, CDCl3) δ ppm 2.24 (s, 3H) 2.28 (s, 6H) 3.44 (s, 2H).

후처리

  1. filtrationThe precipitate was filtered
  2. washwashed with AcOH
  3. extractionextracted twice with 100 mL EtOAc
  4. washwashed once with brine
  5. dry with materialdried over sodium sulfate
  6. customAfter removing the solvent

출처 및 근거

ORD 기록
ord-9e80dedb3cc04bd8a007ce48fc5352ed
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08084479B2

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