Water → HCID 19956225, 화합물

HRID 1779487노트

반응식

HRID 1779487 반응식
P(Cl)(Cl)(Cl)=O.[CH3:6][C:7]1[CH:8]=[CH:9][C:10]([N:16]2[CH:20]=[CH:19][CH:18]=[CH:17]2)=[C:11]([CH:15]=1)[C:12]([OH:14])=O.O>CN(C)C=O>[CH3:6][C:7]1[CH:8]=[CH:9][C:10]2[N:16]3[CH:20]=[CH:19][CH:18]=[C:17]3[C:12](=[O:14])[C:11]=2[CH:15]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 24813Phosphorus oxychlorideHCID 149135585-Methyl-2-(1H-pyrrol-1-yl)benzoic acid

생성물 1

HCID 19956225HCID 19956225, 화합물수율 35%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

At 0° C., add 1.36 ml (14.9 mmol) of phosphorus oxychloride to 1.14 ml (14.9 mmol) of dimethylformamide, then add a solution of 3 g (14.9 mmol) of 5-methyl-2-pyrrol-1-ylbenzoic acid (Preparation 25) in 30 ml of dimethylformamide. After one night's stirring at room temperature, hydrolyse the reaction mixture by pouring into 50 ml of water, extract with 200 ml of diethyl ether, and wash the ethereal phase in succession with water, a saturated aqueous hydrogen carbonate solution and then water. After drying over magnesium sulfate and rendering colourless with animal charcoal, the ethereal phase is concentrated to dryness to yield the title compound.

후처리

  1. extractionextract with 200 ml of diethyl ether
  2. washwash the ethereal phase in succession with water
  3. dry with materialAfter drying over magnesium sulfate and rendering colourless with animal charcoal
  4. concentrationthe ethereal phase is concentrated to dryness

출처 및 근거

ORD 기록
ord-386a5f86a788485f86c1969127f186a0
출처 데이터셋
uspto-grants-1997_05
특허 번호
US05627203

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