Methyl iodide → N-(4-anilinophenyl)-N-(1,3-dimethyl-butyl)-dithiocarbamate methyl ester

HRID 2051583

反応式

HRID 2051583 の反応式
[C:1]1([NH:7][C:8]2[CH:13]=[CH:12][C:11]([NH:14][CH:15]([CH3:20])[CH2:16][CH:17]([CH3:19])[CH3:18])=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:21](=[S:23])=[S:22].[OH-].[Na+].[CH3:26]I>O1CCCC1>[CH3:26][S:22][C:21](=[S:23])[N:14]([C:11]1[CH:12]=[CH:13][C:8]([NH:7][C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[CH:9][CH:10]=1)[CH:15]([CH3:20])[CH2:16][CH:17]([CH3:19])[CH3:18]

参加物

6

反応物 4

HCID 6328Methyl iodideHCID 6348Carbon DisulfideHCID 131011,4-Benzenediamine, N-(1,3-dimethylbutyl)-N'-phenyl-HCID 14798Sodium Hydroxide

生成物 1

HCID 19832493N-(4-anilinophenyl)-N-(1,3-dimethyl-butyl)-dithiocarbamate methyl ester

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

N-phenyl-N'-(1,3-dimethylbutyl)-p-phenylenediamine (26.8g, 0.10 mol) is dissolved in 100 mL tetrahydrofuran in a 250 mL, 3-neck round bottom flask. Carbon disulfide (7.6g, 0.10 mol) is added over 0.5 hours with the concurrent addition of an aqueous solution of sodium hydroxide (4.0g, 0.10 mol). When addition is complete, methyl iodide (14.2g, 0.10 mol) is added and the mixture refluxed for 1 hour. The solvent is then stripped off on a rotary evaporator and the residue extracted with methylene chloride. The extract is dried with MgSO4 and the solvent is again removed on the rotary evaporator to yield the product.

後処理

  1. additionWhen addition
  2. temperaturethe mixture refluxed for 1 hour
  3. customThe solvent is then stripped off on a rotary evaporator
  4. extractionthe residue extracted with methylene chloride
  5. dry with materialThe extract is dried with MgSO4
  6. customthe solvent is again removed on the rotary evaporator
  7. customto yield the product

出典と根拠

ORDレコード
ord-bd7ddee354044392b7d9546781f462db
出典データセット
uspto-grants-1991_05
特許番号
US05019611

関連ノート

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