Iodine → 3-Iodo-2-propynyl butylcarbamate

HRID 404986

反応式

HRID 404986 の反応式
[OH-].[Na+].[CH2:3]([NH:7][C:8](=[O:13])[O:9][CH2:10][C:11]#[CH:12])[CH2:4][CH2:5][CH3:6].[I:14]I.ClCl>CO.O>[CH2:3]([NH:7][C:8](=[O:13])[O:9][CH2:10][C:11]#[C:12][I:14])[CH2:4][CH2:5][CH3:6]

参加物

7

反応物 4

HCID 807IodineHCID 14798Sodium HydroxideHCID 24526ChlorineHCID 108773542-Propynyl butylcarbamate

生成物 1

HCID 620973-Iodo-2-propynyl butylcarbamate収率 166.2%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒2 回

実験手順

At 8° C., 10.1 g of sodium hydroxide (0.244 mol) and 19.0 g of propargyl butylcarbamate (0.122 mol) are introduced as initial charge in 48 g of methanol and 50 g of water. At this temperature, 15.5 g of iodine (0.061 mol) are added in portions. Chlorine (5.6 g, 0.079 mol) is then slowly introduced into the reaction mixture so that the temperature still remains below 8° C. When the metered addition is complete, the mixture is stirred for 1 h at this temperature and then 105 g of water are added. The precipitated solid is isolated by filtration, washed with water and dried in vacuo. This gives 28.5 g of 3-iodo-2-propynyl N-butylcarbamate (purity: 95.0% (HPLC), polyiodized compounds: 0.3% (HPLC), yield: 79%).

後処理

  1. additionWhen the metered addition
  2. customThe precipitated solid is isolated by filtration
  3. washwashed with water
  4. customdried in vacuo

出典と根拠

ORDレコード
ord-afd1f891bba842c0bfed0aeefde76e87
出典データセット
uspto-grants-2014_06
特許番号
US08748652B2

関連ノート

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