Sodium Azide → HCID 178420457, 화합물

HRID 839779

반응식

HRID 839779 반응식
[N-:1]=[N+:2]=[N-:3].[Na+].[C:5]1([N:11]2[CH2:16][CH2:15][N:14]([CH2:17][CH2:18][C:19]#[N:20])[CH2:13][CH2:12]2)[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.Cl.N1CCOCC1>N1CCOCC1>[C:5]1([N:11]2[CH2:12][CH2:13][N:14]([CH2:17][CH2:18][C:19]3[NH:20][N:3]=[N:2][N:1]=3)[CH2:15][CH2:16]2)[CH:6]=[CH:7][CH:8]=[CH:9][CH:10]=1

참가 물질

5

반응물 3

HCID 33557Sodium AzideHCID 197884Morpholine, hydrochloride (1:1)HCID 2583093-(4-Phenylpiperazin-1-yl)propanenitrile

생성물 1

HCID 178420457HCID 178420457, 화합물수율 60%

시약·촉매·용매 1

HCID 8083Morpholine용매

실험 절차

Sodium azide (65 g; 1.0 mol), 4-phenyl-1-(2-cyanoethyl)-piperazine (215 g; 1.0 mol), and morpholine hydrochloride (124 g; 1.0 mol) were dissolved in 1 liter of morpholine, and heated at 120°-125° C with stirring for 4 hours. After the reaction mixture was allowed to cool to room temperature, it was filtered, and the solvent was removed in vacuo. The residue was mixed in water, and the pH of the resulting solution was adjusted to 5. Crude 5-[(4-phenyl-1-piperazyl)ethyl]tetrazole was collected by filtration and was dried; yield -- 170 g. The crude product was recrystallized from water and dried; yield -- 155 g (60% yield; m.p. 190°-194° C).

후처리

  1. temperatureheated at 120°-125° C
  2. filtrationit was filtered
  3. customthe solvent was removed in vacuo
  4. additionThe residue was mixed in water
  5. filtrationCrude 5-[(4-phenyl-1-piperazyl)ethyl]tetrazole was collected by filtration
  6. customwas dried
  7. customThe crude product was recrystallized from water
  8. customdried

출처 및 근거

ORD 기록
ord-5592581d8e494062af45e3245fc2fc98
출처 데이터셋
uspto-grants-1978_06
특허 번호
US04097479

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