1,1'-Carbonyldiimidazole → 5-[2-[2H-1,3-benzooxazine-2,4(3H)-dion-3-yl]ethylthio]imidazo[1,2-a]pyridine

HRID 1081727

반응식

HRID 1081727 반응식
[OH:1][C:2]1[CH:22]=[CH:21][CH:20]=[CH:19][C:3]=1[C:4]([NH:6][CH2:7][CH2:8][S:9][C:10]1[N:15]2[CH:16]=[CH:17][N:18]=[C:14]2[CH:13]=[CH:12][CH:11]=1)=[O:5].[C:23](N1C=CN=C1)(N1C=CN=C1)=[O:24]>O1CCCC1>[O:1]1[C:2]2[CH:22]=[CH:21][CH:20]=[CH:19][C:3]=2[C:4](=[O:5])[N:6]([CH2:7][CH2:8][S:9][C:10]2[N:15]3[CH:16]=[CH:17][N:18]=[C:14]3[CH:13]=[CH:12][CH:11]=2)[C:23]1=[O:24]

참가 물질

4

반응물 2

HCID 682631,1'-CarbonyldiimidazoleHCID 233629775-[2-[2-(Hydroxy)benzoylamino]ethylthio]imidazo[1,2-a]pyridine

생성물 1

HCID 233628185-[2-[2H-1,3-benzooxazine-2,4(3H)-dion-3-yl]ethylthio]imidazo[1,2-a]pyridine수율 77.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 5-[2-[2-(hydroxy)benzoylamino]ethylthio]imidazo[1,2-a]pyridine (627 mg, 2.00 mmoles) in dry tetrahydrofuran (30 ml) was added 1,1'-carbonyldiimidazole (649 mg, 4.00 mmoles) and the mixture was stirred at room temperature for 15 hours. After the solvent was distilled off, chloroform was added to the residue, which was washed with water and dried over anhydrous magnesium sulfate. After the solvent was distilled off, the residue was purified by column chromatography (eluent:ethyl acetate) to obtain 528 mg of the desired product (77.8%, colorless crystals).

후처리

  1. distillationAfter the solvent was distilled off
  2. additionchloroform was added to the residue, which
  3. washwas washed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationAfter the solvent was distilled off
  6. customthe residue was purified by column chromatography (eluent:ethyl acetate)

출처 및 근거

ORD 기록
ord-a8774755c3ad4ebca874b2db5e22891b
출처 데이터셋
uspto-grants-1996_12
특허 번호
US05587383

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