Water → Ethyl cyano-[[[2'-[[[(dimethylamino)methylene]amino]sulfonyl](1,1'-biphenyl)4-yl]methyl](1-oxopentyl)amino]acetate

HRID 260549노트

반응식

HRID 260549 반응식
[NH2:1][C:2](SC)=[C:3]([N:9]([CH2:16][C:17]1[CH:22]=[CH:21][C:20]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=2[S:29]([NH:32][C:33]([NH:35][CH2:36]CC)=O)(=[O:31])=[O:30])=[CH:19][CH:18]=1)[C:10](=[O:15])[CH2:11][CH2:12][CH2:13][CH3:14])[C:4]([O:6][CH2:7][CH3:8])=[O:5].O.[CH3:42]OC>C(O)CO.S(=O)(=O)(O)O>[C:2]([CH:3]([N:9]([CH2:16][C:17]1[CH:18]=[CH:19][C:20]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=2[S:29]([N:32]=[CH:33][N:35]([CH3:36])[CH3:42])(=[O:30])=[O:31])=[CH:21][CH:22]=1)[C:10](=[O:15])[CH2:11][CH2:12][CH2:13][CH3:14])[C:4]([O:6][CH2:7][CH3:8])=[O:5])#[N:1]

참가 물질

6

반응물 3

HCID 962WaterHCID 8254Dimethyl EtherHCID 67741886Ethyl 3-amino-2-[[[2'-[[[(propylamino)-carbonyl]-amino]sulfonyl]-(1,1'-biphenyl)-4-yl]-methyl]-(1-oxopentyl)-amino]-3-(methylthio)-2-propenoate

생성물 1

HCID 53759157Ethyl cyano-[[[2'-[[[(dimethylamino)methylene]amino]sulfonyl](1,1'-biphenyl)4-yl]methyl](1-oxopentyl)amino]acetate

시약·촉매·용매 2

HCID 174Ethylene Glycol용매HCID 1118Sulfuric Acid용매

실험 절차

200 mg of the product of Stage C of Example 3 were dissolved in 5 ml of dimethyl ether of ethylene glycol and 1 ml of concentrated sulfuric acid was added at ambient temperature. After stirring for one hour, water was added while cooling in an ice bath. Extraction was carried out with dichloromethane and the organic phases .were washed and dried. The solvent was evaporated under reduced pressure to obtain 180 mg of crude product which was crystallized from ethyl acetate to obtain 140 mg of the expected product melting at 130°-132° C.

후처리

  1. additionwas added at ambient temperature
  2. temperaturewhile cooling in an ice bath
  3. extractionExtraction
  4. washthe organic phases .were washed
  5. customdried
  6. customThe solvent was evaporated under reduced pressure
  7. customto obtain 180 mg of crude product which
  8. customwas crystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-9d6528f1b5d2408c8239e2f067ec4f57
출처 데이터셋
uspto-grants-1996_06
특허 번호
US05527919

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