Triethylamine → N,N'-diheptyl-S-ethyl-N-propane sulfonyl isothiourea

HRID 2198456ノート

反応式

HRID 2198456 の反応式
C(N(CC)CC)C.[CH2:8]([NH:15][C:16](=[N:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27])[S:17][CH2:18][CH3:19])[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14].[CH2:28]([S:31](Cl)(=[O:33])=[O:32])[CH2:29][CH3:30]>C(Cl)Cl>[CH2:21]([N:20]([S:31]([CH2:28][CH2:29][CH3:30])(=[O:33])=[O:32])[C:16](=[N:15][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14])[S:17][CH2:18][CH3:19])[CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 662791-Propanesulfonyl chlorideHCID 13064686HCID 13064686、化合物

生成物 1

HCID 13079260N,N'-diheptyl-S-ethyl-N-propane sulfonyl isothiourea

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

1.8 g (0.018 mole) of triethylamine was added to 4.5 g (0.015 mole) N,N'-diheptyl-S-ethyl-isothiourea in 50 ml methylene chloride in a stirred round bottom flask. A solution of propanesulfonyl chloride (0.018 mole, 2.6 g) in 8 ml methylene chloride was added dropwise to the above solution at 0° C. The mixture was stirred 1.5 hours at room temperature then at 30°-35° C. for 1.5 hours. The cooled solution was washed twice with 20 ml water, once with 25 ml saturated sodium bicarbonate solution and twice more with 20 ml of water. The organic phase was dried over magnesium sulfate and evaporated invacuo to yield the product as a yellow oil. nD30 1.4805. Yield was 5.2 g (85.4% of theory). The structure was confirmed by IR spectrum. Compound No. 203 in Table I.

後処理

  1. waitat 30°-35° C. for 1.5 hours
  2. washThe cooled solution was washed twice with 20 ml water, once with 25 ml saturated sodium bicarbonate solution and twice more with 20 ml of water
  3. dry with materialThe organic phase was dried over magnesium sulfate
  4. customevaporated invacuo

出典と根拠

ORDレコード
ord-5ea2983ce71e40aa80f43d2239cfb9e0
出典データセット
uspto-grants-1982_11
特許番号
US04357351

反応ノート

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