Methyl iodide → methyl N'-(4-cyanophenyl)carbamimidothioate

HRID 270623ノート

反応式

HRID 270623 の反応式
I[CH3:2].[C:3]([C:5]1[CH:10]=[CH:9][C:8]([NH:11][C:12]([NH2:14])=[S:13])=[CH:7][CH:6]=1)#[N:4]>CC(C)=O>[C:3]([C:5]1[CH:6]=[CH:7][C:8]([N:11]=[C:12]([S:13][CH3:2])[NH2:14])=[CH:9][CH:10]=1)#[N:4]

参加物

4

反応物 2

HCID 6328Methyl iodideHCID 2757973(4-Cyanophenyl)thiourea

生成物 1

HCID 13748458methyl N'-(4-cyanophenyl)carbamimidothioate収率 84%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

Iodomethane (1.76 ml) was added to 4-cyanophenyl-thiourea (5.0 g) in acetone (100 ml). The reaction mixture was stirred overnight at RT. The precipitate was filtered off, dried and dissolved in DCM. The organic solution was washed with NH3 (aq.) (excess), dried with potassium carbonate, filtered, and the solvent was evaporated, yielding 4.53 g (84%, white solid) of methyl N′-(4-cyanophenyl)-carbamimidothioate (intermediate 6).

後処理

  1. filtrationThe precipitate was filtered off
  2. customdried
  3. dissolutiondissolved in DCM
  4. washThe organic solution was washed with NH3 (aq.) (excess)
  5. dry with materialdried with potassium carbonate
  6. filtrationfiltered
  7. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-cc177943ede343319750c72a1105e24b
出典データセット
uspto-grants-2008_11
特許番号
US07449575B2

反応ノート

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