Tetrahydrofuran → HCID 57901756, 화합물

HRID 1851455노트

반응식

HRID 1851455 반응식
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[S:6]([NH:9][C:10]1[CH:11]=[CH:12][CH:13]=[C:14]2[C:18]=1[NH:17][C:16]([C:19](OCC)=[O:20])=[CH:15]2)(=[O:8])=[O:7].O1CCCC1.[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl-].[NH4+]>C(O)C>[OH:20][CH2:19][C:16]1[NH:17][C:18]2[C:14]([CH:15]=1)=[CH:13][CH:12]=[CH:11][C:10]=2[NH:9][S:6]([C:2]1[S:1][CH:5]=[CH:4][CH:3]=1)(=[O:8])=[O:7]

참가 물질

6

반응물 4

HCID 8028TetrahydrofuranHCID 25517Ammonium ChlorideHCID 4076385HCID 4076385, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 57901756HCID 57901756, 화합물수율 82.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a mixture of ethyl 7-[(2-thienylsulfonyl)amino]-1H-indole-2-carboxylate (0.76 g) and tetrahydrofuran (15 mL) was added lithium aluminum hydride (0.15 g) at 0° C., and the mixture was stirred at room temperature for 1 hr. To the reaction mixture was added ethanol (5 mL), and saturated aqueous ammonium chloride solution (0.5 mL) was added. The resulting inorganic salt was removed by filtration, and the filtrate was concentrated. The residue was subjected to silica gel column chromatography, and the title compound (0.55 g, yield 82%) was obtained as colorless crystals from a fraction eluted with ethyl acetate-hexane (1:2, volume ratio). melting point>173° C. (decomposition).

후처리

  1. additionwas added
  2. customThe resulting inorganic salt was removed by filtration
  3. concentrationthe filtrate was concentrated

출처 및 근거

ORD 기록
ord-34746676f09d48ce9a9797f4b30e755d
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08957070B2

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