N-Iodosuccinimide → HCID 178432598, 화합물

HRID 1488033노트

반응식

HRID 1488033 반응식
C1C(=O)N([I:8])C(=O)C1.[CH3:9][C:10]1[N:11]=[C:12]([C:15]2([CH3:19])[CH2:18][O:17][CH2:16]2)[NH:13][CH:14]=1>C(#N)C>[I:8][C:14]1[NH:13][C:12]([C:15]2([CH3:19])[CH2:16][O:17][CH2:18]2)=[N:11][C:10]=1[CH3:9]

참가 물질

4

반응물 2

HCID 120273N-IodosuccinimideHCID 178430849HCID 178430849, 화합물2회

생성물 1

HCID 178432598HCID 178432598, 화합물수율 93.2%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

NIS (2.61 g, 11.58 mmol) was added portion-wise to a solution of 4-methyl-2-(3-methyloxetan-3-yl)-1H-imidazole (compound 175.1, 1.76 g, 11.58 mmol) in acetonitrile (60 mL). The mixture was stirred at room temperature for 1 hour, then was partitioned between EtOAc (300 mL) and water (80 mL). The organic layer was washed with saturated sodium thiosulfate (50 mL), brine (50 mL), dried (MgSO4) and concentrated under reduced pressure to give the title compound as a light yellow solid (3.0 g, 93%). m/z (ES+) 279 (M+H)+.

후처리

  1. customwas partitioned between EtOAc (300 mL) and water (80 mL)
  2. washThe organic layer was washed with saturated sodium thiosulfate (50 mL), brine (50 mL)
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-4e71dc75488c42a486dd9af1e0e78679
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09428502B2

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