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Methyl iodide → HCID 14801186、化合物

HRID 476528
ノート
印刷プレビュー

反応式

HRID 476528 の反応式
[CH3:1][O:2][CH2:3][C:4]1[C:5]([CH3:14])=[C:6]([CH:8]=[CH:9][C:10]=1[S:11][C:12]#N)[NH2:7].O.O.O.O.O.O.O.O.O.[S-2].[Na+].[Na+].CI>C(O)C>[CH3:1][O:2][CH2:3][C:4]1[C:5]([CH3:14])=[C:6]([CH:8]=[CH:9][C:10]=1[S:11][CH3:12])[NH2:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 73972Sodium sulfide nonahydrateHCID 14801185HCID 14801185、化合物

生成物 1

HCID 14801186HCID 14801186、化合物収率 92.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

29.1 g (0.14 mol) of 3-methoxymethyl-2-methyl-4-thiocyanoaniline was dissolved in 200 ml of ethanol and mixed with 100 ml of an aqueous solution containing 33.6 g of sodium sulfide nonahydrate at room temperature. Then, 21.9 g of methyl iodide was dropwise added thereto, and the mixture was reacted at room temperature for 3 hours. After completion of the reaction, the solvent was distilled off under reduced pressure, and water and chloroform were added to the residue. Then, the organic layer was separated and washed sequentially with water and a saturated sodium chloride aqueous solution and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain 25.6 g of the desired product as an oily substance.

後処理

  1. customthe mixture was reacted at room temperature for 3 hours
  2. customAfter completion of the reaction
  3. distillationthe solvent was distilled off under reduced pressure, and water and chloroform
  4. additionwere added to the residue
  5. customThen, the organic layer was separated
  6. washwashed sequentially with water
  7. dry with materiala saturated sodium chloride aqueous solution and then dried over anhydrous sodium sulfate
  8. distillationThe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-e3e89dfb60ef41889c6f048df7245669
出典データセット
uspto-grants-1989_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04885022

反応ノート

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