Acetone → Methyl 2-chloro-6-fluorobenzthioimidate hydroiodide

HRID 2269659

반응식

HRID 2269659 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 18347932Methyl 2-chloro-6-fluorobenzthioimidate hydroiodide수율 46.9%

시약·촉매·용매 1

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

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-67d5220cc59c4cfab38fbd25bef74308
출처 데이터셋
uspto-grants-2001_12
특허 번호
US06329528B1

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