Tetrahydrofuran → HCID 136060812, 화합물

HRID 1851522노트

반응식

HRID 1851522 반응식
[CH3:1][C:2]1[N:3]=[C:4]([C:12]2[NH:13][C:14]3[C:19]([CH:20]=2)=[CH:18][CH:17]=[CH:16][C:15]=3[NH:21][S:22]([C:25]2[S:26][CH:27]=[CH:28][CH:29]=2)(=[O:24])=[O:23])[S:5][C:6]=1[C:7]([O:9]CC)=[O:8].[OH-].[Na+].O1CCCC1>CO>[CH3:1][C:2]1[N:3]=[C:4]([C:12]2[NH:13][C:14]3[C:19]([CH:20]=2)=[CH:18][CH:17]=[CH:16][C:15]=3[NH:21][S:22]([C:25]2[S:26][CH:27]=[CH:28][CH:29]=2)(=[O:24])=[O:23])[S:5][C:6]=1[C:7]([OH:9])=[O:8]

참가 물질

5

반응물 3

HCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 136060809HCID 136060809, 화합물

생성물 1

HCID 136060812HCID 136060812, 화합물수율 44%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
60 °C

실험 절차

A mixture of ethyl 4-methyl-2-{7-[(2-thienylsulfonyl)amino]-1H-indol-2-yl}-1,3-thiazole-5-carboxylate (0.42 g), 8N aqueous sodium hydroxide solution (0.4 mL), tetrahydrofuran (6 mL) and methanol (6 mL) was stirred at 60° C. for 1 hr. The reaction mixture was concentrated, and water was added to the residue. The mixture was acidified with 10% aqueous citric acid solution, and the resulting crystals were filtrated, washed with water and dried. The obtained crystals were dissolved in tetrahydrofuran, treated with activated carbon, and concentrated to give the title compound (0.17 g, yield 44%) as yellow crystals. The crystals were recrystallized from ethyl acetate-hexane. melting point>253° C. (decomposition).

후처리

  1. concentrationThe reaction mixture was concentrated
  2. additionwater was added to the residue
  3. filtrationthe resulting crystals were filtrated
  4. washwashed with water
  5. customdried
  6. dissolutionThe obtained crystals were dissolved in tetrahydrofuran
  7. additiontreated with activated carbon
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-d32ab5e37c1c4fcd88dad7f1940b9322
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08957070B2

반응 노트

불러오는 중…