Tetrahydrofuran → HCID 57901756、化合物

HRID 1851455ノート

反応式

HRID 1851455 の反応式
[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]

参加物

6

反応物 4

HCID 8028TetrahydrofuranHCID 25517Ammonium ChlorideHCID 4076385HCID 4076385、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 57901756HCID 57901756、化合物収率 82.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-34746676f09d48ce9a9797f4b30e755d
出典データセット
uspto-grants-2015_02
特許番号
US08957070B2

反応ノート

読み込み中…