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

HRID 2198456노트

반응식

HRID 2198456 반응식
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]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 662791-Propanesulfonyl chlorideHCID 13064686HCID 13064686, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5ea2983ce71e40aa80f43d2239cfb9e0
출처 데이터셋
uspto-grants-1982_11
특허 번호
US04357351

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