Triethylamine → HCID 51042118、化合物

HRID 17456ノート

反応式

HRID 17456 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]([C:8]2[C:9](F)=[C:10]3[O:14][C:13]([CH:15]4[CH2:17][CH2:16]4)=[N:12][C:11]3=[C:18]([C:21]#[N:22])[C:19]=2[CH3:20])[CH:5]=[CH:6][CH:7]=1.C(N(CC)CC)C.[CH3:31][N:32]([CH3:38])[C@H:33]1[CH2:37][CH2:36][NH:35][CH2:34]1.C(=O)([O-])O.[Na+]>CS(C)=O.C(OCC)(=O)C>[NH2:1][C:2]1[CH:3]=[C:4]([C:8]2[C:9]([N:35]3[CH2:36][CH2:37][C@H:33]([N:32]([CH3:38])[CH3:31])[CH2:34]3)=[C:10]3[O:14][C:13]([CH:15]4[CH2:17][CH2:16]4)=[N:12][C:11]3=[C:18]([C:21]#[N:22])[C:19]=2[CH3:20])[CH:5]=[CH:6][CH:7]=1

参加物

7

反応物 4

HCID 8471TriethylamineHCID 516892Sodium BicarbonateHCID 7019156(3S)-(-)-3-(Dimethylamino)pyrrolidineHCID 685845026-(3-Aminophenyl)-2-cyclopropyl-7-fluoro-5-methyl-1,3-benzoxazole-4-carbonitrile

生成物 1

HCID 51042118HCID 51042118、化合物

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
90 °C

実験手順

6-(3-Aminophenyl)-2-cyclopropyl-7-fluoro-5-methyl-1,3-benzoxazole-4-carbonitrile (I-178) (200 mg, 0.65 mmol) was dissolved in dimethyl sulfoxide (4 ml), then at room temperature, triethylamine (136 μl, 0.98 mmol) and (3S)-3-(dimethylamino)pyrrolidine (124 μl, 0.98 mmol) were added. The solution was stirred under nitrogen atmosphere at 90° C. for 19 hours, then cooled to room temperature. This was fractionated with ethyl acetate and an aqueous saturated sodium hydrogencarbonate solution.

後処理

  1. temperaturecooled to room temperature

出典と根拠

ORDレコード
ord-902a9ff84aca45ca9c38902439cd98a2
出典データセット
uspto-grants-2010_06
特許番号
US07737166B2

反応ノート

読み込み中…