3-Cyano-7-hydroxy-4-methylcoumarin → HCID 136387768, 화합물

HRID 579438노트

반응식

HRID 579438 반응식
[OH:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([CH3:15])=[C:7]([C:13]#[N:14])[C:8](=[O:12])[O:9]2)=[CH:4][CH:3]=1.[NH4+]=[S:17]>CN(C)C=O>[OH:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([CH3:15])=[C:7]([C:13](=[S:17])[NH2:14])[C:8](=[O:12])[O:9]2)=[CH:4][CH:3]=1

참가 물질

3

반응물 1

HCID 53931723-Cyano-7-hydroxy-4-methylcoumarin

생성물 1

HCID 136387768HCID 136387768, 화합물수율 36.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 7-Hydroxy-4-methyl-2-oxo-2H-chromene-3-carbonitrile (7.50 g, 37.31 mmol) in N,N-dimethylformamide (150 mL), ammonium sulfide (40-48 wt. % solution in water; 38 mL, 560 mmol) was added, and the resulted mixture was stirred at room temperature for a week. An additional portion of ammonium sulfide (38 mL) was added on every second day. The solution was evaporated and the solid residue was triturated with water, filtered and dried. The obtained crude product was purified by column chromatography (Kieselgel 60), with chloroform-methanol (1:1) as eluent. The title compound (3.20 g, 13.6 mmol, 36%) was isolated as a yellow powder,

후처리

  1. customThe solution was evaporated
  2. customthe solid residue was triturated with water
  3. filtrationfiltered
  4. customdried
  5. customThe obtained crude product
  6. customwas purified by column chromatography (Kieselgel 60), with chloroform-methanol (1:1) as eluent

출처 및 근거

ORD 기록
ord-30b67dfb2de145eeaae157fb6a32826c
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09040714B2

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