Hydrochloric Acid → 8-iodo-2,3,4,5-tetrahydro-1H-1-benzazepine-2,5-dione

HRID 1892170노트

반응식

HRID 1892170 반응식
[I:1][C:2]1[CH:18]=[CH:17][C:5]2[C:6](=[O:16])[CH:7](C(OC)=O)[CH2:8][C:9](=[O:11])[NH:10][C:4]=2[CH:3]=1.Cl>CS(C)=O.O>[I:1][C:2]1[CH:18]=[CH:17][C:5]2[C:6](=[O:16])[CH2:7][CH2:8][C:9](=[O:11])[NH:10][C:4]=2[CH:3]=1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 58476574methyl 8-iodo-2,5-dioxo-2,3,4,5-tetrahydro-1H-1-benzazepine-4-carboxylate

생성물 1

HCID 584766238-iodo-2,3,4,5-tetrahydro-1H-1-benzazepine-2,5-dione수율 99.6%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 962Water용매

반응 조건

온도
150 °C

실험 절차

A mixture of methyl 8-iodo-2,5-dioxo-2,3,4,5-tetrahydro-1H-1-benzazepine-4-carboxylate (74 g, 0.2 mol) in DMSO (560 mL) and H2O (16 mL) was heated at 150° C. for 4 h. The reaction mixture was allowed to cool to rt, ice (1.0 L) was added, and the mixture was allowed to stir 12 h. To the flask was added 1N HCl (1.0 L) at 0° C. and the mixture allowed to stir for 3 h. The resulting precipitate was filtered and dried under reduced pressure to afford 8-iodo-3,4-dihydro-1H-1-benzazepine-2,5-dione (60 g, 97%).

후처리

  1. temperatureto cool to rt
  2. stirringto stir for 3 h
  3. filtrationThe resulting precipitate was filtered
  4. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-ae9e583168924d1399debeefe1474848
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08507667B2

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