Anisole → HCID 178470514、化合物

HRID 1794683ノート

反応式

HRID 1794683 の反応式
C1(OC)C=CC=CC=1.COC1C=CC(C[N:16]2[C:20]([C:21]([O:23][CH2:24][CH3:25])=[O:22])=[C:19]([C:26](=[O:40])[C:27]3[CH:32]=[C:31]([O:33][CH3:34])[C:30]([O:35][CH3:36])=[CH:29][C:28]=3[N+:37]([O-:39])=[O:38])[N:18]=[N:17]2)=CC=1.COC1C=CC(CN2C(C(=O)C3C=C(OC)C(OC)=CC=3[N+]([O-])=O)=C(C(OCC)=O)N=N2)=CC=1>FC(F)(F)C(O)=O>[CH3:36][O:35][C:30]1[C:31]([O:33][CH3:34])=[CH:32][C:27]([C:26]([C:19]2[NH:18][N:17]=[N:16][C:20]=2[C:21]([O:23][CH2:24][CH3:25])=[O:22])=[O:40])=[C:28]([N+:37]([O-:39])=[O:38])[CH:29]=1

参加物

5

反応物 3

HCID 7519AnisoleHCID 22222563Ethyl 1-(4-methoxybenzyl)-5-(4,5-dimethoxy-2-nitrobenzoyl)-1,2,3-triazole-4-carboxylateHCID 22222639ethyl 1-(4-methoxybenzyl)-4-(4,5-dimethoxy-2-nitrobenzoyl)-1H-1,2,3-triazole-5-carboxylate

生成物 1

HCID 178470514HCID 178470514、化合物収率 95.2%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

反応条件

温度
60 °C

実験手順

Anisole (1 ml) was added to a solution of an about 1:1 mixture (4.4 g) of ethyl 1-(4-methoxybenzyl)-4-(4,5-dimethoxy-2-nitrobenzoyl)-1H-1,2,3-triazole-5-carboxylate (Synthesis Example 1, b-1) and ethyl 1-(4-methoxybenzyl)-5-(4,5-dimethoxy-2-nitrobenzoyl)-1H-1,2,3-triazole-4-carboxylate(Synthesis Example 1, b-2) in trifluoroacetic acid (10 ml), and the mixture was stirred at 60° C. for 10 hr. After the mixture was allowed to stand for cooling, the solvent was evaporated under reduced pressure, followed by azeotropic evaporation using toluene. The resultant crystal was collected by filtration, washed with diethyl ether, and then dried to give ethyl 5-(4,5-dimethoxy-2-nitrobenzoyl)-1H-1,2,3-triazole-4-carboxylate (3.12 g, 95%).

後処理

  1. temperaturefor cooling
  2. customthe solvent was evaporated under reduced pressure
  3. customfollowed by azeotropic evaporation
  4. filtrationThe resultant crystal was collected by filtration
  5. washwashed with diethyl ether
  6. customdried

出典と根拠

ORDレコード
ord-45f272dfcf1c4f3aaa16b9d43e8b97cc
出典データセット
uspto-grants-2006_04
特許番号
US07022860B2

反応ノート

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