Hydrochloric Acid → HCID 178441131, 화합물

HRID 1440414노트

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HRID 1440414 반응식
[C:1]([C:5]1[CH:6]=[C:7]([CH:17]=[C:18]([C:21]([CH3:24])([CH3:23])[CH3:22])[C:19]=1[OH:20])[NH:8][C:9]1[CH:10]=[C:11]([CH:14]=[CH:15][CH:16]=1)[C:12]#[N:13])([CH3:4])([CH3:3])[CH3:2].[N-:25]=[N+:26]=[N-:27].[Na+].[Cl-].[NH4+].[Cl-].[Li+].Cl>CN(C)C=O>[C:1]([C:5]1[CH:6]=[C:7]([CH:17]=[C:18]([C:21]([CH3:24])([CH3:23])[CH3:22])[C:19]=1[OH:20])[NH:8][C:9]1[CH:10]=[C:11]([C:12]2[NH:27][N:26]=[N:25][N:13]=2)[CH:14]=[CH:15][CH:16]=1)([CH3:4])([CH3:3])[CH3:2]

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 433294Lithium ChlorideHCID 224015743-(3,5-Di-t-butyl-4-hydroxyanilino)benzonitrile

생성물 1

HCID 178441131HCID 178441131, 화합물수율 65.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
110 °C

실험 절차

Eight g (0.025 mole) of 3-(3,5-di-t-butyl-4-hydroxyanilino)benzonitrile (from Example 27), 4.9 g (0.075 mole) of sodium azide, 4.0 g (0.075 mole) of ammonium chloride, 1.06 g (0.025 mole) of lithium chloride and 60 ml of N,N-dimethylformamide were combined under a nitrogen atmosphere and heated at 110° C. for 48 hours. The reaction mixture was poured into cold 6N hydrochloric acid and a gummy solid precipitated out. The supernatant was decanted off and the residue dissolved in ethanol. The ethanol solution was diluted with water and a pink solid was collected. This material was recrystallized from a mixture of ethanol and water to give 5.97 g of 5-[3-(3,5-di-t-butyl-4-hydroxyanilino)phenyl]tetrazole, m.p. 231°-233° C. Analysis: Calculated for C21H27N5O: % C, 69.0; % H, 7.4; % N, 19.2; Found: % C, 68.4; % H, 7.6; % N, 18.8.

후처리

  1. customa gummy solid precipitated out
  2. customThe supernatant was decanted off
  3. dissolutionthe residue dissolved in ethanol
  4. additionThe ethanol solution was diluted with water
  5. customa pink solid was collected
  6. customThis material was recrystallized from a mixture of ethanol and water

출처 및 근거

ORD 기록
ord-dac6be3b10824f8b8cf6e808807603f8
출처 데이터셋
uspto-grants-1996_03
특허 번호
US05498745

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