Hydrochloric Acid → 1,3,4,5-Tetrahydro-3-(methoxycarbonyl)-4-(methoxyphenyl)-7-(trifluoromethyl)-2H-1-benzazepin-2-one

HRID 580396

반응식

HRID 580396 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][C:3]=1[CH2:12][CH:13]([CH:22]([C:27](OC)=[O:28])[C:23]([O:25][CH3:26])=[O:24])[C:14]1[CH:19]=[CH:18][C:17](OC)=[CH:16][CH:15]=1.[CH3:31][O-:32].[Na+].Cl>CO>[CH3:26][O:25][C:23]([CH:22]1[CH:13]([C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:19]=2[O:32][CH3:31])[CH2:12][C:3]2[CH:4]=[C:5]([C:8]([F:10])([F:11])[F:9])[CH:6]=[CH:7][C:2]=2[NH:1][C:27]1=[O:28])=[O:24]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 10942334Sodium MethoxideHCID 14156191[2-(2-Amino-5-trifluoromethylphenyl)-1-(4-methoxyphenyl)ethyl]propanedioic acid, dimethyl ester

생성물 1

HCID 201350951,3,4,5-Tetrahydro-3-(methoxycarbonyl)-4-(methoxyphenyl)-7-(trifluoromethyl)-2H-1-benzazepin-2-one

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

Under an argon atmosphere, a stirred solution of [2-(2-amino-5-trifluoromethylphenyl)-1-(4-methoxyphenyl)ethyl]propanedioic acid, dimethyl ester (20.0 g; 0.047 mol) in 200 ml of methanol was treated with 13.3 ml of 25% sodium methoxide in methanol and heated to reflux. After about 2.75 hours of heating, the mixture was cooled in ice water and 1N hydrochloric acid was added to precipitate the product. Stirring in an ice water bath, followed by filtering, washing with water and air-drying yielded 19.0 g of product. The product was suspended in 30 ml of isopropanol, allowed to stand for one hour, filtered and washed with isopropanol and hexane to yield 13.64 g of the title compound, melting point 161°-163° C.

후처리

  1. temperatureheated to reflux
  2. temperatureAfter about 2.75 hours of heating
  3. customto precipitate the product
  4. filtrationby filtering
  5. washwashing with water
  6. customair-drying

출처 및 근거

ORD 기록
ord-80bd263374444c00baf3854d6360a708
출처 데이터셋
uspto-grants-1988_06
특허 번호
US04752645

연결된 노트

불러오는 중…