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Chloroacetyl isocyanate → 1H-Imidazole-2-methanol, 5-((3,5-dichlorophenyl)thio)-4-(1-methylethyl)-1-(3-quinolinylmethyl)-, carbamate (ester)

HRID 1416054
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HRID 1416054 반응식
[OH:1][CH2:2][C:3]1[N:4]([CH2:20][C:21]2[CH:22]=[N:23][C:24]3[C:29]([CH:30]=2)=[CH:28][CH:27]=[CH:26][CH:25]=3)[C:5]([S:11][C:12]2[CH:17]=[C:16]([Cl:18])[CH:15]=[C:14]([Cl:19])[CH:13]=2)=[C:6]([CH:8]([CH3:10])[CH3:9])[N:7]=1.ClC[C:33]([N:35]=C=O)=[O:34].C(=O)(O)[O-].[Na+]>O1CCCC1.CO.[Zn]>[C:33]([O:1][CH2:2][C:3]1[N:4]([CH2:20][C:21]2[CH:22]=[N:23][C:24]3[C:29]([CH:30]=2)=[CH:28][CH:27]=[CH:26][CH:25]=3)[C:5]([S:11][C:12]2[CH:17]=[C:16]([Cl:18])[CH:15]=[C:14]([Cl:19])[CH:13]=2)=[C:6]([CH:8]([CH3:10])[CH3:9])[N:7]=1)(=[O:34])[NH2:35]
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참가 물질

7

반응물 3

HCID 78209Chloroacetyl isocyanateHCID 4740441H-Imidazole-2-methanol, 5-((3,5-dichlorophenyl)thio)-4-(1-methylethyl)-1-(3-quinolinylmethyl)-HCID 516892Sodium Bicarbonate2회

생성물 1

HCID 4740451H-Imidazole-2-methanol, 5-((3,5-dichlorophenyl)thio)-4-(1-methylethyl)-1-(3-quinolinylmethyl)-, carbamate (ester)수율 78%

시약·촉매·용매 3

HCID 23994
Zinc
촉매
HCID 887Methanol용매
HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

In 5 ml of tetrahydrofuran was dissolved 223 mg (0.50 mmol)of 2-hydroxymethyl-5-(3,5-dichlorophenylthio)-4-isopropyl-1-(quinolin-3-ylmethyl)-1H-imidazole (109), followed by dropwise addition of 72 mg (0.60 mmol)of chloroacetylisocyanate with stirring at 0° C., and the mixture was stirred at room temperature for 30 minutes. After the reaction completion, the mixture was worked up. To the reaction mixture was added a saturated aqueous sodium bicarbonate solution, extracted with methylene chloride, the extract was washed with water and dried. The-solvent was distilled off under reduced pressure, and 2-chloroacetyl-carbamoyloxymethyl-5-(3,5-dichlorophenylthio)-4-isopropyl-1-(quinolin-3-ylmethyl)-1H-imidazole (110)suited to the next step of the reaction was obtained. mp 167-170° C. The crystals were dissolved in 20 ml of aqueous methanol, 40 mg of Zn powder was added, and the mixture was stirred at room temperature for 5 hours. After the reaction completion, the mixture was worked up. To the reaction mixture was added a saturated aqueous sodium hydrogen carbonate solution, and the insoluble material was removed by filtration under reduced pressure through Celite. The filtrate was concentrated, extracted with methylene chloride, the extract was washed with water and dried, and the solvent was distilled off. The residual crystals were washed with ethyl acetate and ether to give 195 mg of Compound I-128 (yield 78%). mp 214-216° C.

후처리

  1. stirringthe mixture was stirred at room temperature for 30 minutes
  2. extractionextracted with methylene chloride
  3. washthe extract was washed with water
  4. customdried
  5. distillationThe-solvent was distilled off under reduced pressure, and 2-chloroacetyl-carbamoyloxymethyl-5-(3,5-dichlorophenylthio)-4-isopropyl-1-(quinolin-3-ylmethyl)-1H-imidazole (110)suited to the next step of the reaction
  6. customwas obtained
  7. stirringthe mixture was stirred at room temperature for 5 hours
  8. customthe insoluble material was removed by filtration under reduced pressure through Celite
  9. concentrationThe filtrate was concentrated
  10. extractionextracted with methylene chloride
  11. washthe extract was washed with water
  12. customdried
  13. distillationthe solvent was distilled off
  14. washThe residual crystals were washed with ethyl acetate and ether

출처 및 근거

ORD 기록
ord-ebd997c20c4047e99c009324b4d8db96
출처 데이터셋
uspto-grants-1999_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05910506

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