Hydrochloric Acid → N-(2-Cyano-4-oxo-4H-chromen-8-yl)-4-(4-phenylbutoxy)benzamide

HRID 2258283노트

반응식

HRID 2258283 반응식
C(C1C=CC(C)=NC=1)C.[C:10]1([CH2:16][CH2:17][CH2:18][CH2:19][O:20][C:21]2[CH:43]=[CH:42][C:24]([C:25]([NH:27][C:28]3[C:37]4[O:36][C:35]([C:38](=O)[NH2:39])=[CH:34][C:33](=[O:41])[C:32]=4[CH:31]=[CH:30][CH:29]=3)=[O:26])=[CH:23][CH:22]=2)[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.Cl>C1(C)C=CC=CC=1>[C:10]1([CH2:16][CH2:17][CH2:18][CH2:19][O:20][C:21]2[CH:22]=[CH:23][C:24]([C:25]([NH:27][C:28]3[C:37]4[O:36][C:35]([C:38]#[N:39])=[CH:34][C:33](=[O:41])[C:32]=4[CH:31]=[CH:30][CH:29]=3)=[O:26])=[CH:42][CH:43]=2)[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 77285-Ethyl-2-methylpyridineHCID 10895736Pranlukast Chromene Carboxamide Impurity

생성물 1

HCID 9911011N-(2-Cyano-4-oxo-4H-chromen-8-yl)-4-(4-phenylbutoxy)benzamide수율 87.5%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To a mixture containing 50 g of 5-ethyl-2-methylpyridine and 50 g of toluene was added 10 g of 8-[4-(4-phenyl-1-butoxy)benzoyl]amino-2-carbamoyl-4-oxo-4H-benzopyran, and the reaction was allowed to proceed at 60° C. for 6 hours. After completion of the reaction, 400 ml of 4N hydrochloric acid was added, and the mixture was extracted with 400 ml of toluene. The extract was washed with diluted hydrochloric acid, water and aqueous sodium hydrogencarbonate, and the organic layer was concentrated under reduced pressure, which afforded 8.4 g of 8-[4-(4-phenyl-1-butoxy) benzoyl]amino-2-cyano-4-oxo-4H-benzopyran as a pale brown product (yield 88%).

후처리

  1. additionwas added
  2. extractionthe mixture was extracted with 400 ml of toluene
  3. washThe extract was washed with diluted hydrochloric acid, water and aqueous sodium hydrogencarbonate
  4. concentrationthe organic layer was concentrated under reduced pressure, which

출처 및 근거

ORD 기록
ord-d42e5dac722a4ca1bae042f08d3b7255
출처 데이터셋
uspto-grants-1997_08
특허 번호
US05659051

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