Sodium Azide → HCID 178518972, 화합물

HRID 260893노트

반응식

HRID 260893 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[N-:5]=[N+:6]=[N-:7].[Na+].[Cl:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[N:16]=[C:17]=[O:18].N([O-])=O.[Na+]>O.O1CCCC1>[CH:13]1[CH:12]=[C:11]([N:16]2[NH:7][N:6]=[N:5][C:17]2=[O:18])[C:10]([Cl:9])=[CH:15][CH:14]=1

참가 물질

7

반응물 4

HCID 33557Sodium AzideHCID 76833Chlorophenyl isocyanateHCID 6451240Aluminum(III) ChlorideHCID 23668193Sodium Nitrite

생성물 1

HCID 178518972HCID 178518972, 화합물수율 25.5%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

Anhydrous aluminum chloride (1.5 g) was added to tetrahydrofuran (30 ml) with ice bath cooling and the resulting mixture was stirred for fifteen minutes. To the mixture was added sodium azide (0.65 g) and 2-chlorophenylisocyanate (1.53 g), followed by a sixteen hour-refluxing. After cooling, the reaction mixture was added with stirring to a mixture of sodium nitrite (1 g), water (200 ml) and ice (100 g) and the resulting mixture was worked up in the same way as in Comparative Synthesis Example 1 to obtain the desired 1-(2-chlorophenyl)-5(4H)-tetrazolinone (0.5 g) having a m.p. in the range of from 124.5° to 125.5° C. in a yield of 25% of theory.

후처리

  1. temperaturecooling
  2. waitfollowed by a sixteen hour
  3. temperature-refluxing
  4. temperatureAfter cooling
  5. additionthe reaction mixture was added
  6. customthe resulting mixture was worked up in the same way as in Comparative Synthesis Example 1

출처 및 근거

ORD 기록
ord-689c11898bfd4c73a8f35e5c0e15b267
출처 데이터셋
uspto-grants-1996_06
특허 번호
US05530135

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