Toluene → HCID 59135737、化合物

HRID 504962ノート

反応式

HRID 504962 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](=[S:21])[NH2:20])=[CH:15]2)(=[O:8])=[O:7].[C:22]([O:27][CH2:28][CH3:29])(=[O:26])[C:23]#[C:24][CH3:25].C(P(CCCC)CCCC)CCC.C1(C)C=CC=CC=1>O1CCCC1>[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]1[S:21][CH:24]([CH2:23][C:22]([O:27][CH2:28][CH3:29])=[O:26])[CH2:25][N:20]=1)=[CH:15]2)(=[O:7])=[O:8]

参加物

6

反応物 4

HCID 1140TolueneHCID 13831TributylphosphineHCID 78043Ethyl 2-butynoate2 回HCID 57901763HCID 57901763、化合物

生成物 1

HCID 59135737HCID 59135737、化合物収率 28%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
60 °C

実験手順

A solution of 7-[(2-thienylsulfonyl)amino]-1H-indole-2-carbothioamide (4.3 g), ethyl but-2-ynoate (3.2 mL) and tributylphosphine (3.2 mL) in tetrahydrofuran (40 mL)-toluene (40 mL) was stirred at room temperature for 2 days. ethyl but-2-ynoate (1.6 mL) was added to the reaction solution again, and the mixture was stirred at 60° C. for 2 hr. The reaction solution was concentrated under reduced pressure, and the obtained residue was subjected to silica gel column chromatography (ethyl acetate:hexane=2:8-4:6) to give the title compound (1.6 g, yield: 28%) as a pale-brown oil.

後処理

  1. concentrationThe reaction solution was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-46afffb057bc4624aecc1b9f1e063716
出典データセット
uspto-grants-2010_08
特許番号
US07777047B2

反応ノート

読み込み中…