Methyl iodide → HCID 178504010、化合物

HRID 1803181ノート

反応式

HRID 1803181 の反応式
[I:1][CH3:2].[CH3:3][C:4]1[N:8]=[C:7]([CH3:9])[N:6]([C:10]2[CH:15]=[CH:14][C:13]([NH:16][C:17]([NH2:19])=[S:18])=[CH:12][C:11]=2[F:20])[N:5]=1>C(O)C>[IH:1].[CH3:3][C:4]1[N:8]=[C:7]([CH3:9])[N:6]([C:10]2[CH:15]=[CH:14][C:13]([NH:16][C:17]([S:18][CH3:2])=[NH:19])=[CH:12][C:11]=2[F:20])[N:5]=1

参加物

4

反応物 2

HCID 6328Methyl iodideHCID 866499211-(4-(3,5-dimethyl-1H-1,2,4-triazol-1-yl)-3-fluorophenyl)thiourea

生成物 1

HCID 178504010HCID 178504010、化合物収率 101%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
70 °C

実験手順

Step T (4) [80456-011]: Iodomethane (0.281 mL, 4.51 mmol) was added to a solution of 1-(4-(3,5-dimethyl-1H-1,2,4-triazol-1-yl)-3-fluorophenyl)thiourea (1.14 g, 4.30 mmol) in absolute ethanol (50 mL). The resulting mixture was heated at 70° C. for 3 h. After cooling to rt, the reaction was concentrated in vacuo. The residual volatiles were removed under high vacuum to afford methyl 4-(3,5-dimethyl-1H-1,2,4-triazol-1-yl)-3-fluorophenylcarbamimidothioate, hydroiodide (1.76 g, 4.32 mmol, 101% yield) as a grey solid. LC-MS (M+H)+ 280.1.

後処理

  1. temperatureAfter cooling to rt
  2. concentrationthe reaction was concentrated in vacuo
  3. customThe residual volatiles were removed under high vacuum

出典と根拠

ORDレコード
ord-d61490e222424db29d6b6156fbb211cc
出典データセット
uspto-grants-2013_01
特許番号
US08349880B2

反応ノート

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