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Water → 1-Trityl-1,2,4-triazole-3-carboxylic acid ethyl ester

HRID 2307538
ノート
印刷プレビュー

反応式

HRID 2307538 の反応式
[CH2:1]([O:3][C:4]([C:6]1[N:10]=[CH:9][NH:8][N:7]=1)=[O:5])[CH3:2].C(N(CC)C(C)C)(C)C.[C:20](Cl)([C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1)([C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.O>CN(C=O)C.C(OC(=O)C)C>[CH2:1]([O:3][C:4]([C:6]1[N:10]=[CH:9][N:8]([C:20]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)([C:33]2[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=2)[C:27]2[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=2)[N:7]=1)=[O:5])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962WaterHCID 6456Trityl chlorideHCID 81531DiisopropylethylamineHCID 178418794HCID 178418794、化合物

生成物 1

HCID 574241681-Trityl-1,2,4-triazole-3-carboxylic acid ethyl ester収率 43%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

In 60 ml of DMF was dissolved 7.62 g (54 mmol) of 1H-1,2,4-triazole-3-carboxylic acid ethyl ester. To the solution were added at room temperature 14 g (108 mmol) of N,N-diisopropylethylamine and 15.8 g (56.7 mmol) of tritylchloride. The mixture was stirred for 2 hours. 300 ml of water and 300 ml of ethylacetate were added thereto. The crystal was filtered, dissolved in 150 ml of chloroform, washed with water and dried. The solvent was removed. The residue was crystallized from ether to give 8.91 g of the titled compound. The ethylacetate layer was washed with water, dried and evaporated. The residue was crystallized from ether to give 4.73 g of the titled compound. 13.64 g of 1-trityl-1,2,4-triazole-3-carboxylic acid ethyl ester was totally obtained. Yield: 66%.

後処理

  1. filtrationThe crystal was filtered
  2. dissolutiondissolved in 150 ml of chloroform
  3. washwashed with water
  4. customdried
  5. customThe solvent was removed
  6. customThe residue was crystallized from ether

出典と根拠

ORDレコード
ord-f1877809efc24161ad45332422070b69
出典データセット
uspto-grants-2004_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06831177B1

反応ノート

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