Triethylamine → 1-[4-[4-(4-Hexyloxyphenyl)piperazin-1-yl]benzoyloxy]benzotriazole

HRID 351553ノート

反応式

HRID 351553 の反応式
[OH:1][N:2]1[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[N:4]=[N:3]1.Cl.[CH2:12]([O:18][C:19]1[CH:24]=[CH:23][C:22]([N:25]2[CH2:30][CH2:29][N:28]([C:31]3[CH:39]=[CH:38][C:34]([C:35](O)=[O:36])=[CH:33][CH:32]=3)[CH2:27][CH2:26]2)=[CH:21][CH:20]=1)[CH2:13][CH2:14][CH2:15][CH2:16][CH3:17].C(N(CC)CC)C.Cl.C(N=C=NCCCN(C)C)C>O.ClCCl>[CH2:12]([O:18][C:19]1[CH:20]=[CH:21][C:22]([N:25]2[CH2:26][CH2:27][N:28]([C:31]3[CH:39]=[CH:38][C:34]([C:35]([O:1][N:2]4[C:6]5[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=5[N:4]=[N:3]4)=[O:36])=[CH:33][CH:32]=3)[CH2:29][CH2:30]2)=[CH:23][CH:24]=1)[CH2:13][CH2:14][CH2:15][CH2:16][CH3:17]

参加物

7

反応物 4

HCID 8471TriethylamineHCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 698180334-[4-(4-Hexyloxyphenyl)piperazin-1-yl]benzoic acid hydrochloride

生成物 1

HCID 227132451-[4-[4-(4-Hexyloxyphenyl)piperazin-1-yl]benzoyloxy]benzotriazole収率 93.8%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 1-hydroxybenzotriazole (5.35 g) and 4-[4-(4-hexyloxyphenyl)piperazin-1-yl]benzoic acid hydrochloride (15 g) in the mixture of triethylamine (9.64 ml) and dichloromethane (450 ml) was added 1-ethyl-3-(3′-dimethylaminopropyl) carbodiimide hydrochloride (WSCD.HCl) (12.6 g) and stirred for 4 hours at ambient temperature. The reaction mixture was added to water. The organic layer was taken and dried over magnesium sulfate. Magnesium sulfate was filtered off, and the filtrate was evaporated under reduced pressure to give 1-[4-[4-(4-hexyloxyphenyl)piperazin-1-yl]benzoyloxy]benzotriazole (16.78 g).

後処理

  1. dry with materialdried over magnesium sulfate
  2. filtrationMagnesium sulfate was filtered off
  3. customthe filtrate was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-1394ded476814c2bb9f1ccf9d009a025
出典データセット
uspto-grants-2004_06
特許番号
US06743776B2

反応ノート

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