Acetic Acid → Methyl 2-[5-bromo-2-(4-methanesulfonylphenyl)thiophen-3-yl]acetate

HRID 2199575노트

반응식

HRID 2199575 반응식
C1C(=O)N([Br:8])C(=O)C1.[CH3:9][S:10]([C:13]1[CH:18]=[CH:17][C:16]([C:19]2[S:20][CH:21]=[CH:22][C:23]=2[CH2:24][C:25]([O:27][CH3:28])=[O:26])=[CH:15][CH:14]=1)(=[O:12])=[O:11].CC(O)=O>CO.C(Cl)(Cl)Cl>[Br:8][C:21]1[S:20][C:19]([C:16]2[CH:15]=[CH:14][C:13]([S:10]([CH3:9])(=[O:12])=[O:11])=[CH:18][CH:17]=2)=[C:23]([CH2:24][C:25]([O:27][CH3:28])=[O:26])[CH:22]=1

참가 물질

6

반응물 3

HCID 176Acetic Acid2회HCID 67184N-bromobutanimide3회HCID 71230756Methyl 2-[2-(4-methanesulfonylphenyl)thiophen-3-yl]acetate2회

생성물 1

HCID 71230633Methyl 2-[5-bromo-2-(4-methanesulfonylphenyl)thiophen-3-yl]acetate

시약·촉매·용매 2

HCID 887Methanol용매2회HCID 6212Chloroform용매2회

반응 조건

온도
0 °C

실험 절차

NBS (209 mg, 1.18 mmol) was added in small portions to a stirred solution of Intermediate Y (365 mg, 1.18 mmol) in a mixture of MeOH (10 ml) and chloroform (5 ml) at 0° C. AcOH (0.250 ml) was added and the reaction was stirred at 0° C. for 1 hour then at r.t. for 3 hours. More NBS (35 mg, 0.20 mmol) was added at 0° C. and the reaction was stirred at r.t. over night. A new reaction was also started. NBS (342 mg, 1.92 mmol) was added in small portions to a stirred solution of Intermediate Y (519 mg, 1.67 mmol) in a mixture of MeOH (15 ml) and chloroform (7 ml) at 0° C. AcOH (0.50 ml) was added and the reaction was stirred at r.t. over night.

후처리

  1. waitat r.t. for 3 hours
  2. stirringthe reaction was stirred at r.t. over night
  3. customA new reaction
  4. stirringthe reaction was stirred at r.t. over night

출처 및 근거

ORD 기록
ord-a153574c1492456483680e7e878b5fcc
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09359311B2

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