Water → 7-Iodo-3,4-dihydro-1H-benzo[b]azepine-2,5-dione

HRID 544984노트

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HRID 544984 반응식
[I:1][C:2]1[CH:19]=[CH:18][C:5]2[NH:6][C:7](=[O:17])[CH2:8][CH:9](C(OCC)=O)[C:10](=[O:11])[C:4]=2[CH:3]=1.[Na+].[Cl-].O>CS(C)=O>[I:1][C:2]1[CH:19]=[CH:18][C:5]2[NH:6][C:7](=[O:17])[CH2:8][CH2:9][C:10](=[O:11])[C:4]=2[CH:3]=1

참가 물질

5

반응물 3

HCID 962Water2회HCID 5234Sodium ChlorideHCID 66934628ethyl 7-iodo-2,5-dioxo-2,3,4,5-tetrahydro-1H-benzo[b]azepine-4-carboxylate

생성물 1

HCID 120121827-Iodo-3,4-dihydro-1H-benzo[b]azepine-2,5-dione

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

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온도
150 °C

실험 절차

To a solution of ethyl 7-iodo-2,5-dioxo-2,3,4,5-tetrahydro-1H-benzo[b]azepine-4-carboxylate (iii-a) (4.84 g, 13.2 mmol) in dimethyl sulfoxide (66 mL) was added a solution of NaCl (81 mg, 15.9 mmol) in H2O (475 μL, 26.4 mmol). The reaction mixture was heated to 150° C. for 2 h, and subsequently cooled to 0° C. for 30 min. H2O (120 mL) was added and the solution was allowed to stir for an additional 1.5 h at 0° C. The resulting precipitate was filtered to provide iv-a (3.2 g, 81%) as a purple/brown solid: MS m/z=302 (M+H).

후처리

  1. temperaturesubsequently cooled to 0° C. for 30 min
  2. filtrationThe resulting precipitate was filtered
  3. customto provide iv-a (3.2 g, 81%) as a purple/brown solid

출처 및 근거

ORD 기록
ord-3d8bc9ee549d4e2a94908e927eee9005
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07935694B2

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