Methyl iodide → 11-{[(Methylsulfanyl)carbonothioyl]amino}undecanoic acid

HRID 895062ノート

反応式

HRID 895062 の反応式
[OH-].[K+].[NH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][C:14]([OH:16])=[O:15].[C:17](=[S:19])=[S:18].[CH3:20]I>C(O)C.O>[C:14]([CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][NH:3][C:17](=[S:19])[S:18][CH3:20])([OH:16])=[O:15]

参加物

7

反応物 4

HCID 6328Methyl iodideHCID 6348Carbon DisulfideHCID 14797Potassium HydroxideHCID 1708311-Aminoundecanoic acid

生成物 1

HCID 2057407811-{[(Methylsulfanyl)carbonothioyl]amino}undecanoic acid

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒2 回HCID 962Water溶媒

実験手順

A suspension of 56 g. (1.0 mol.) of potassium hydroxide and 100 g. (0.5 mol.) of 11-aminoundecanoic acid in 170 ml. of water was stirred for 30 minutes at 25° then 40 g. (0.52 mol.) of carbon disulfide and 80 ml. of ethanol were added and the reaction mixture was stirred at 25° for 12 hours. The mixture was refluxed gently for two hours and cooled. Methyl iodide (71 g., 0.3 mol.) and 130 ml. of ethanol were added to the mixture and it was stirred at 25° for 12 hours. The mixture was evaporated to remove the ethanol and the solid residue was collected by filtration to give methyl 10-carboxydecyldithiocarbamate.

後処理

  1. additionA suspension of 56 g
  2. temperatureThe mixture was refluxed gently for two hours
  3. temperaturecooled
  4. stirringwas stirred at 25° for 12 hours
  5. customThe mixture was evaporated
  6. customto remove the ethanol
  7. filtrationthe solid residue was collected by filtration

出典と根拠

ORDレコード
ord-db84e434b31947b8be3aa552ed8cbb27
出典データセット
uspto-grants-1981_08
特許番号
US04286089

反応ノート

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