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1,1'-Carbonyldiimidazole → 4-{2-[2-(Acetylamino)-1,3-thiazol-4-yl]ethyl}phenyl tert-butyl hydrazine-1,2-dicarboxylate

HRID 1892470
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HRID 1892470 반응식
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][C:10]2[N:11]=[C:12]([NH:15][C:16](=[O:18])[CH3:17])[S:13][CH:14]=2)=[CH:4][CH:3]=1.[C:19]([N:26]1C=CN=C1)(N1C=CN=C1)=[O:20].[C:31]([O:35][C:36]([CH3:39])([CH3:38])[CH3:37])(=[O:34])[NH:32]N>O1CCCC1>[NH:26]([C:19]([O:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][C:10]2[N:11]=[C:12]([NH:15][C:16](=[O:18])[CH3:17])[S:13][CH:14]=2)=[CH:4][CH:3]=1)=[O:20])[NH:32][C:31]([O:35][C:36]([CH3:39])([CH3:38])[CH3:37])=[O:34]
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5

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HCID 682631,1'-CarbonyldiimidazoleHCID 70091tert-Butyl carbazateHCID 86649977N-{4-[2-(4-hydroxyphenyl)ethyl]-1,3-thiazol-2-yl}acetamide

생성물 1

HCID 866499784-{2-[2-(Acetylamino)-1,3-thiazol-4-yl]ethyl}phenyl tert-butyl hydrazine-1,2-dicarboxylate수율 50.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
45 °C

실험 절차

To a solution of N-{4-[2-(4-hydroxyphenyl)ethyl]-1,3-thiazol-2-yl}acetamide (655.8 mg, 2.50 mmol) in anhydrous tetrahydrofuran (12 ml) was added 1,1′-carbonyldiimidazole (608.1 mg, 3.75 mmol). After stirring at 45° C. for 1 hr, the mixture was cooled to room temperature. tert-Butyl carbazate (495.6 mg, 3.75 mmol) was added, and the mixture was stirred at room temperature for 15 hr. The reaction mixture was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (FUJI SILYSIA CHEMICAL LTD. BW-300SP 80 g, ethyl acetate:hexane=1:1→3:2) and chemically modified silica gel column chromatography (FUJI SILYSIA CHEMICAL LTD. DM-2035 45 g, dichloromethane:methanol=50:1→20:1) to give 4-{2-[2-(acetylamino)-1,3-thiazol-4-yl]ethyl}phenyl tert-butyl hydrazine-1,2-dicarboxylate (526.4 mg, 1.252 mmol, yield 50.0%) as a white solid.

후처리

  1. temperaturethe mixture was cooled to room temperature
  2. stirringthe mixture was stirred at room temperature for 15 hr
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. customthe residue was purified by silica gel column chromatography (FUJI SILYSIA CHEMICAL LTD. BW-300SP 80 g, ethyl acetate:hexane=1:1→3:2) and chemically modified silica gel column chromatography (FUJI SILYSIA CHEMICAL LTD. DM-2035 45 g, dichloromethane:methanol=50:1→20:1)

출처 및 근거

ORD 기록
ord-3a66605e2c9245dabcf0c70e190a4e5d
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08507690B2

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