Methyl Isocyanate → N-methyl-2-{2-[2-(4-phenylpiperazin-1-yl)ethyloxy]phenyl}thiazolidine-3-carboxamide

HRID 1789350노트

반응식

HRID 1789350 반응식
[C:1]1([N:7]2[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][O:15][C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[CH:22]3[NH:26][CH2:25][CH2:24][S:23]3)[CH2:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:27][N:28]=[C:29]=[O:30]>O1CCCC1>[CH3:27][NH:28][C:29]([N:26]1[CH2:25][CH2:24][S:23][CH:22]1[C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=1[O:15][CH2:14][CH2:13][N:10]1[CH2:11][CH2:12][N:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[CH2:8][CH2:9]1)=[O:30]

참가 물질

4

반응물 2

HCID 12228Methyl IsocyanateHCID 137680992-{2-[2-(4-Phenylpiperazin-1-yl)ethyloxy]phenyl}thiazolidine

생성물 1

HCID 13767927N-methyl-2-{2-[2-(4-phenylpiperazin-1-yl)ethyloxy]phenyl}thiazolidine-3-carboxamide수율 89.7%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

3.69 g of 2-{2-[2-(4-phenylpiperazin-1-yl)ethyloxy]phenyl}thiazolidine are dissolved in 40 ml of tetrahydrofuran, and 0.62 g of methyl isocyanate is added thereto at room temperature. The mixture is stirred at the same temperature for 2 hours. The mixture is concentrated under reduced pressure to remove solvent. Water is added to the residue, and crystalline precipitates are collected by filtration. The crystals are washed with ethanol and ether, and then recrystallized from a mixture of ethyl acetate and n-hexane. 3.82 g of N-methyl-2-{2-[2-(4-phenylpiperazin-1-yl)ethyloxy]phenyl}thiazolidin-3-carboxamide are obtained. Yield: 89.7%.

후처리

  1. customat room temperature
  2. concentrationThe mixture is concentrated under reduced pressure
  3. customto remove solvent
  4. additionWater is added to the residue
  5. customcrystalline precipitates
  6. filtrationare collected by filtration
  7. washThe crystals are washed with ethanol and ether
  8. customrecrystallized from a mixture of ethyl acetate and n-hexane

출처 및 근거

ORD 기록
ord-cf2b730c091b4f5fb5ea937a4065d490
출처 데이터셋
uspto-grants-1987_08
특허 번호
US04689327

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