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Water → HCID 178505113, 화합물

HRID 866880
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HRID 866880 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

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

생성물 1

HCID 178505113HCID 178505113, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-ed6ee3a967bd4b89a6bff7bd3895eb53
출처 데이터셋
uspto-grants-1978_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04101656

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