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Potassium Hydroxide → potassium 2-(4-methoxybenzyl)-2H-tetrazole-5-carboxylate

HRID 325738
ノート
印刷プレビュー

反応式

HRID 325738 の反応式
COC1C=CC(CN2C(C(OCC)=O)=NN=N2)=CC=1.[CH3:20][O:21][C:22]1[CH:38]=[CH:37][C:25]([CH2:26][N:27]2[N:31]=[N:30][C:29]([C:32]([O:34]CC)=[O:33])=[N:28]2)=[CH:24][CH:23]=1.S1(CCCC1)(=O)=O.[OH-].[K+:47]>C(O)C.O>[CH3:20][O:21][C:22]1[CH:23]=[CH:24][C:25]([CH2:26][N:27]2[N:31]=[N:30][C:29]([C:32]([O-:34])=[O:33])=[N:28]2)=[CH:37][CH:38]=1.[K+:47]
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 14797Potassium HydroxideHCID 31347SulfolaneHCID 11097352ethyl 1-(4-methoxybenzyl)-1H-tetrazole-5-carboxylateHCID 13596243ethyl 2-(4-methoxybenzyl)-2H-tetrazole-5-carboxylate

生成物 1

HCID 23677909potassium 2-(4-methoxybenzyl)-2H-tetrazole-5-carboxylate収率 35.4%

試薬・触媒・溶媒 2

HCID 702
Ethanol
溶媒
HCID 962Water溶媒

実験手順

A mixture of ethyl 1-(4-methoxybenzyl)-1H-tetrazole-5-carboxylate and ethyl 2-(4-methoxybenzyl)-2H-tetrazole-5-carboxylate (11.7 g) (prepared as described below and still containing a little sulpholane) was dissolved in hot ethanol (165 ml) and the solution was treated with a solution of potassium hydroxide (4.5 g) in water (13.5 ml). The mixture was cooled and the white crystalline solid which separated was filtered off to give potassium 2-(4-methoxybenzyl)-2H-tetrazole-5-carboxylate (4.3 g), m.p. 271°-273° C. (with decomposition). [The pure salt, obtained as a hemihydrate after recrystallisation from water, had a melting point of 273°-274° C. (with decomposition)].

後処理

  1. customprepared
  2. temperatureThe mixture was cooled
  3. customthe white crystalline solid which separated
  4. filtrationwas filtered off

出典と根拠

ORDレコード
ord-a3da7f7cff57400b8998478f56beea94
出典データセット
uspto-grants-1984_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04442115

反応ノート

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