Hydrochloric Acid → HCID 66758458, 화합물

HRID 1507869노트

반응식

HRID 1507869 반응식
[NH2:1][C:2]1[S:3][C:4]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)=[CH:5][C:6]=1[C:7]([O:9]CC)=O.[C:19](#[N:21])[CH3:20].Cl>O1CCOCC1>[F:18][C:15]1[CH:14]=[CH:13][C:12]([C:4]2[S:3][C:2]3[N:1]=[C:19]([CH3:20])[NH:21][C:7](=[O:9])[C:6]=3[CH:5]=2)=[CH:17][CH:16]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 6342AcetonitrileHCID 21529229Ethyl 2-amino-5-(4-fluorophenyl)thiophene-3-carboxylate

생성물 1

HCID 66758458HCID 66758458, 화합물수율 98.6%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

To a solution of ethyl 2-amino-5-(4-fluorophenyl)thiophene-3-carboxylate (0.3 g, 1.13 mmol) and acetonitrile (0.56 ml, 11.3 mmol) in dioxane (4 ml) was added 4M HCl in dioxane (4 ml). The mixture was stirred at room temperature overnight. The solvents were removed under reduced pressure. The residue was diluted with water and made alcaline with a saturated aqueous sodium bicarbonate solution. The precipitate was filtered off, washed with water and dried. The crude residue was purified by flash chromatography on silica gel (CH2Cl2/MeOH 60:1) to yield the title compound as a white solid (0.29 g, 81%).

후처리

  1. customThe solvents were removed under reduced pressure
  2. additionThe residue was diluted with water
  3. filtrationThe precipitate was filtered off
  4. washwashed with water
  5. customdried
  6. customThe crude residue was purified by flash chromatography on silica gel (CH2Cl2/MeOH 60:1)

출처 및 근거

ORD 기록
ord-09aa14ecb4f74aeb908e2d987912a610
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09221822B2

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