N-Iodosuccinimide → HCID 178432598、化合物

HRID 1488033ノート

反応式

HRID 1488033 の反応式
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]

参加物

4

反応物 2

HCID 120273N-IodosuccinimideHCID 178430849HCID 178430849、化合物2 回

生成物 1

HCID 178432598HCID 178432598、化合物収率 93.2%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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)+.

後処理

  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

出典と根拠

ORDレコード
ord-4e71dc75488c42a486dd9af1e0e78679
出典データセット
uspto-grants-2016_08
特許番号
US09428502B2

反応ノート

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