Water → 3-(1-methyl-3-indolyl)-4-[1-[3-(1-methyl-5-tetrazolylthio)propyl]-3-indolyl]-1H-pyrrole-2,5-dione

HRID 1421190노트

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HRID 1421190 반응식
[CH3:1][N:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]([C:11]2[C:12](=[O:34])[NH:13][C:14](=[O:33])[C:15]=2[C:16]2[C:24]3[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=3)[N:18]([CH2:25][CH2:26][CH2:27]OS(C)(=O)=O)[CH:17]=2)=[CH:3]1.[Na].[SH:36][C:37]1[N:41]([CH3:42])[N:40]=[N:39][N:38]=1.O>CS(C)=O>[CH3:1][N:2]1[C:10]2[C:9](=[CH:8][CH:7]=[CH:6][CH:5]=2)[C:4]([C:11]2[C:12](=[O:34])[NH:13][C:14](=[O:33])[C:15]=2[C:16]2[C:24]3[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=3)[N:18]([CH2:25][CH2:26][CH2:27][S:36][C:37]3[N:41]([CH3:42])[N:40]=[N:39][N:38]=3)[CH:17]=2)=[CH:3]1

참가 물질

5

반응물 3

HCID 962WaterHCID 151630513-(1-methyl-3-indolyl)-4-[1-[3-(methylsulphonyloxy)propyl]-3-indolyl]-1H-pyrrole-2,5-dioneHCID 178482029HCID 178482029, 화합물

생성물 1

HCID 187803003-(1-methyl-3-indolyl)-4-[1-[3-(1-methyl-5-tetrazolylthio)propyl]-3-indolyl]-1H-pyrrole-2,5-dione수율 46.1%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

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온도
55 °C

실험 절차

100 mg of the product of Example 58 in 10 ml of DMSO were treated with 120 mg of 5-mercapto-1-methyltetrazole sodium salt. The solution was heated at 55° C. for 6 hours, then cooled and poured into water. The aqueous phase was extracted with ethyl acetate. The ethyl acetate extracts were dried and concentrated. Chromatography on silica gel with dichloromethane/ethyl acetate (4:1) gave 48 mg of 3-(1-methyl-3-indolyl)-4-[1-[3-(1-methyl-5-tetrazolylthio)propyl]-3-indolyl]-1H-pyrrole-2,5-dione, m.p. 95°-97° C.

후처리

  1. temperaturecooled
  2. extractionThe aqueous phase was extracted with ethyl acetate
  3. dry with materialThe ethyl acetate extracts were dried
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-be13fdf5ae684c7c99b79605a9e9bc25
출처 데이터셋
uspto-grants-2000_06
특허 번호
USRE036736

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