Acetone → Methyl 2-chloro-6-fluorobenzthioimidate hydroiodide

HRID 2269659ノート

反応式

HRID 2269659 の反応式
[Cl:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([F:11])[C:3]=1[C:4](=[S:6])[NH2:5].[CH3:12]C(C)=O.[I:16]C>C(#N)C.O>[IH:16].[Cl:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([F:11])[C:3]=1[C:4]([S:6][CH3:12])=[NH:5]

参加物

5

反応物 3

HCID 180AcetoneHCID 6328Methyl iodideHCID 77452422-Chloro-6-fluorobenzene-1-carbothioamide

生成物 1

HCID 18347932Methyl 2-chloro-6-fluorobenzthioimidate hydroiodide収率 46.9%

試薬・触媒・溶媒 1

HCID 18373917Acetonitrile--water (1/1)溶媒

実験手順

Into a 50 mL three necked round bottom flask equipped with a magnetic stirrer was added 2-chloro-6-fluorobenzthioamide (3.78 g, 20 mmol) and acetone (20 mL). Dropwise was added iodomethane (2.84 g, 1.24 mL, 20 mmol) and the mixture was allowed to stir at room temperature overnight with monitoring via HPCL (60/40 acetonitrile/water). The solids were removed via filtration and washed with small portions of acetone to give methyl 2-chloro-6-fluorobenzthioimidate hydroiodide as a light yellow solid: 3.1 g (46.9% yield): 1H NMR (DMSO-d6) δ7.7 (m, 1H), 7.5 (m, 2H), 2.7 (s, 3H).

後処理

  1. customThe solids were removed via filtration
  2. washwashed with small portions of acetone

出典と根拠

ORDレコード
ord-67d5220cc59c4cfab38fbd25bef74308
出典データセット
uspto-grants-2001_12
特許番号
US06329528B1

反応ノート

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