Ammonium Chloride → HCID 178420853, 화합물

HRID 437592노트

반응식

HRID 437592 반응식
[CH:1]1[CH:5]=[C:4]([S:6][CH2:7][C:8]#[N:9])[S:3][CH:2]=1.[N-:10]=[N+:11]=[N-:12].[Na+].[Cl-].[NH4+].[Cl-].[Li+]>CN(C)C=O>[S:3]1[CH:2]=[CH:1][CH:5]=[C:4]1[S:6][CH2:7][C:8]1[NH:12][N:11]=[N:10][N:9]=1

참가 물질

6

반응물 4

HCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 433294Lithium ChlorideHCID 21429205(2-Thienylthio)acetonitrile

생성물 1

HCID 178420853HCID 178420853, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 7.76 g. (50 millimoles) of thiophene-2-thioacetonitrile, 4.30 g. (66 millimoles) of sodium azide, 3.55 g. (66 millimoles) of ammonium chloride, and 0.38 g. (9 millimoles) of lithium chloride is maintained for 5 hours at 120° in 50 ml. of dry dimethylformamide. The dimethylformamide is withdrawn under vacuum, the residue is combined with 500 ml. of cold 0.2 N sodium hydroxide solution and extracted with ether. The aqueous phase is adjusted to pH 3 and extracted three times with respectively 150 ml. of ether. The ether phase yields, after drying (Na2SO4) and concentration, the crude, solid tetrazole which is recrystallized once from acetonitrile/water and once from ethanol/water.

후처리

  1. additionA mixture of 7.76 g
  2. customThe dimethylformamide is withdrawn under vacuum
  3. extractionof cold 0.2 N sodium hydroxide solution and extracted with ether
  4. extractionextracted three times with respectively 150 ml
  5. customThe ether phase yields
  6. customafter drying
  7. concentration(Na2SO4) and concentration
  8. customthe crude, solid tetrazole which is recrystallized once from acetonitrile/water and once from ethanol/water

출처 및 근거

ORD 기록
ord-bb604464a8444790a08ece4b8de05e57
출처 데이터셋
uspto-grants-1977_06
특허 번호
US04031236

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