Dimethyl Sulfoxide → 2-Amino-nicotinic acid N'-(2-(4-benzyloxy-phenyl)-acetyl)-hydrazide

HRID 1927231ノート

反応式

HRID 1927231 の反応式
CS(C)=O.[CH2:5]([O:12][C:13]1[CH:18]=[CH:17][C:16]([CH2:19][C:20]([NH:22][NH2:23])=[O:21])=[CH:15][CH:14]=1)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[NH2:24][C:25]1[N:33]=[CH:32][CH:31]=[CH:30][C:26]=1[C:27](O)=[O:28].CN([P+](ON1N=NC2C=CC=CC1=2)(N(C)C)N(C)C)C.F[P-](F)(F)(F)(F)F>O.C(N(CC)CC)C>[CH2:5]([O:12][C:13]1[CH:18]=[CH:17][C:16]([CH2:19][C:20]([NH:22][NH:23][C:27](=[O:28])[C:26]2[CH:30]=[CH:31][CH:32]=[N:33][C:25]=2[NH2:24])=[O:21])=[CH:15][CH:14]=1)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1

参加物

7

反応物 4

HCID 679Dimethyl SulfoxideHCID 729302-Aminonicotinic acidHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 59287387(4-Benzyloxy-phenyl)-acetic acid hydrazide

生成物 1

HCID 592873892-Amino-nicotinic acid N'-(2-(4-benzyloxy-phenyl)-acetyl)-hydrazide収率 89.1%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8471Triethylamine溶媒

実験手順

To a solution of DMSO (3 mL) of (4-benzyloxy-phenyl)-acetic acid hydrazide (130 mg) described in Manufacturing Example 8-1 were added triethylamine (0.21 mL), 2-aminonicotinic acid (70 mg), and BOP reagent (benzotriazol-1-yloxytris(dimethylamino)phosphonium hexafluorophosphate) (250 mg), which was stirred for 1 hour at the same temperature. Water was added to the reaction solution, and the solids thus precipitated were filtered off to obtain the titled compound (170 mg).

後処理

  1. customthe solids thus precipitated
  2. filtrationwere filtered off

出典と根拠

ORDレコード
ord-c4b0f9293ee745e0bd242867d9106980
出典データセット
uspto-grants-2012_05
特許番号
US08183264B2

反応ノート

読み込み中…