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HCID 13596127、化合物 → HCID 178521988、化合物

HRID 325717
ノート
印刷プレビュー

反応式

HRID 325717 の反応式
C([N:8]1[C:12]([C:13]([NH:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[O:22]CC2C=CC=CC=2)=[O:14])=[N:11][N:10]=[N:9]1)C1C=CC=CC=1>C(O)(=O)C.[Pd]>[OH:22][C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=1[NH:15][C:13]([C:12]1[NH:11][N:10]=[N:9][N:8]=1)=[O:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 13596127HCID 13596127、化合物

生成物 1

HCID 178521988HCID 178521988、化合物収率 42.3%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 176Acetic Acid溶媒

実験手順

A solution of 1-benzyl-2'-benzyloxy-1H-tetrazole-5-carboxanilide (2.0 g) in glacial acetic acid (100 ml) was hydrogenated at 53° C. and 4.1 kg/cm2 for 18.5 hours, using a catalyst of palladium on charcoal (5% w/w). The mixture was filtered and the filtrate was evaporated at 40° C. in vacuo. The resulting solid was dissolved in a minimum volume of aqueous ammonia solution (2 N). The solution was filtered and then acidified with dilute hydrochloric acid (2 N). The resulting solid was filtered off, dried and recrystallised from aqueous dimethylformamide to give 2'-hydroxytetrazole-5-carboxanilide (0.45 g), m.p. 220°-223° C.

後処理

  1. customwas hydrogenated at 53° C.
  2. filtrationThe mixture was filtered
  3. customthe filtrate was evaporated at 40° C. in vacuo
  4. dissolutionThe resulting solid was dissolved in a minimum volume of aqueous ammonia solution (2 N)
  5. filtrationThe solution was filtered
  6. filtrationThe resulting solid was filtered off
  7. customdried
  8. customrecrystallised from aqueous dimethylformamide

出典と根拠

ORDレコード
ord-2638b32a378041b78a0147fd7a8656a3
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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