Acetic Acid → 9-methoxy-1-oxo-3,4-dihydro-2H-benzothiopheno[2,3-f][1,4]thiazepin-5-one

반응식

[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[S:17][C:10]3[C:11](=[O:16])[NH:12][CH2:13][CH2:14][S:15][C:9]=3[C:7]=2[CH:8]=1.CC(O)=[O:20]>>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[S:17][C:10]3[C:11](=[O:16])[NH:12][CH2:13][CH2:14][S:15](=[O:20])[C:9]=3[C:7]=2[CH:8]=1

참가 물질

반응물 2

HCID 176Acetic Acid

HCID 461195(1)Benzothieno(2,3-f)-1,4-thiazepin-5(2H)-one, 3,4-dihydro-9-methoxy-

생성물 1

HCID 5125479-methoxy-1-oxo-3,4-dihydro-2H-benzothiopheno[2,3-f][1,4]thiazepin-5-one수율 69%

실험 절차

A mixture of 2,3 -dihydro-9 -methoxy-[1]benzothieno [2,3-f]-1,4-thiazepin-5 (4H) -one (200 mg, 0.75 mmol) and NaBO3 -4H2O (116 mg, 0.75 mmol) in 18 mL of AcOH is stirred at room temperature overnight. The reaction mixture is filtered and 60 mL of water is added to the filtrate. Filtration provides 2,3-dihydro-9-methoxy-[1]benzothieno[2,3-f]-1,4-thiazepin-5 (4H) -one-1-oxide in 69% yield, mp 215°-216° C. (dec).

후처리

filtrationThe reaction mixture is filtered
addition60 mL of water is added to the filtrate
filtrationFiltration

출처 및 근거

ORD 기록: ord-0ead350194a243c9ab361d96cce24172
출처 데이터셋: uspto-grants-1997_12
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US05703069

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