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

HRID 325738
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HRID 325738 반응식
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]
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참가 물질

7

반응물 4

HCID 14797Potassium HydroxideHCID 31347SulfolaneHCID 11097352ethyl 1-(4-methoxybenzyl)-1H-tetrazole-5-carboxylateHCID 13596243ethyl 2-(4-methoxybenzyl)-2H-tetrazole-5-carboxylate

생성물 1

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

시약·촉매·용매 2

HCID 702
Ethanol
용매
HCID 962Water용매

실험 절차

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)].

후처리

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

출처 및 근거

ORD 기록
ord-a3da7f7cff57400b8998478f56beea94
출처 데이터셋
uspto-grants-1984_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04442115

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