Trifluoroacetic acid → Ethyl 6-[2-benzyloxy-5-bromobenzylamino]-3-pyridazinecarboxylate

HRID 1455990ノート

反応式

HRID 1455990 の反応式
[CH2:1]([O:8][C:9]1[CH:34]=[CH:33][C:32]([Br:35])=[CH:31][C:10]=1[CH2:11][N:12]([C:20]1[N:25]=[N:24][C:23]([C:26]([O:28][CH2:29][CH3:30])=[O:27])=[CH:22][CH:21]=1)C(OC(C)(C)C)=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.FC(F)(F)C(O)=O>C(Cl)Cl>[CH2:1]([O:8][C:9]1[CH:34]=[CH:33][C:32]([Br:35])=[CH:31][C:10]=1[CH2:11][NH:12][C:20]1[N:25]=[N:24][C:23]([C:26]([O:28][CH2:29][CH3:30])=[O:27])=[CH:22][CH:21]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 22105523Ethyl 6-[N-(2-benzyloxy-5-bromobenzyl)-N-(tert-butoxycarbonyl)amino]-3-pyridazinecarboxylate

生成物 1

HCID 22105509Ethyl 6-[2-benzyloxy-5-bromobenzylamino]-3-pyridazinecarboxylate収率 92%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of ethyl 6-[N-(2-benzyloxy-5-bromobenzyl)-N-(tert-butoxycarbonyl)amino]-3-pyridazinecarboxylate (2.0 g) and trifluoroacetic acid (25 ml) in CH2Cl2 (25 ml) was allowed to stand for 18 hours. The solvents were evaporated, the residue dissolved in CH2Cl2 and washed with dilute aqueous Na2CO3 solution, dried (MgSO4) and evaporated to give ethyl 6-[2-benzyloxy-5-bromobenzylamino]-3-pyridazinecarboxylate as a solid (1.5 g).

後処理

  1. customThe solvents were evaporated
  2. dissolutionthe residue dissolved in CH2Cl2
  3. washwashed with dilute aqueous Na2CO3 solution
  4. dry with materialdried (MgSO4)
  5. customevaporated

出典と根拠

ORDレコード
ord-39b2d114c0544e7c992378c21d71dde2
出典データセット
uspto-grants-1998_12
特許番号
US05843942

反応ノート

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