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Water → HCID 178505113、化合物

HRID 866880
ノート
印刷プレビュー

反応式

HRID 866880 の反応式
[N+](C1C=C([N+]([O-])=O)C=CC=1[S:13][C:14]1[N:18]([CH2:19][CH2:20][NH:21][S:22]([CH3:25])(=[O:24])=[O:23])[N:17]=[N:16][N:15]=1)([O-])=O.C[O-].[Na+].O>CO>[CH3:25][S:22]([NH:21][CH2:20][CH2:19][N:18]1[C:14]([SH:13])=[N:15][N:16]=[N:17]1)(=[O:24])=[O:23]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 10942334Sodium MethoxideHCID 203186985-(2,4-Dinitrophenylthio)-1-(2-methanesulfonamidoethyl)tetrazole

生成物 1

HCID 178505113HCID 178505113、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

5-(2,4-Dinitrophenylthio)-1-(2-methanesulfonamidoethyl)tetrazole (4.46 g, 11.5 mmol) was added to 60 ml of 5% sodium methoxide in methanol. After 1 hour, water was added and the solid material was removed by filtration. The filtrate was concentrated in vacuo and 3N hydrochloric acid was added to the residue to bring the pH to 1.4. The acidic solution was filtered and the filtrate was extracted twice with ethyl acetate. The extracts were combined and concentrated to give a residue which crystallized upon addition of ethyl acetate to give 1-(2-methanesulfonamidoethyl)tetrazole-5-thiol, mp 131°-132°.

後処理

  1. customthe solid material was removed by filtration
  2. concentrationThe filtrate was concentrated in vacuo and 3N hydrochloric acid
  3. additionwas added to the residue
  4. filtrationThe acidic solution was filtered
  5. extractionthe filtrate was extracted twice with ethyl acetate
  6. concentrationconcentrated
  7. customto give a residue which
  8. customcrystallized upon addition of ethyl acetate

出典と根拠

ORDレコード
ord-ed6ee3a967bd4b89a6bff7bd3895eb53
出典データセット
uspto-grants-1978_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04101656

反応ノート

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