Sodium Azide → HCID 178420457、化合物

HRID 839779

反応式

HRID 839779 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 178420457HCID 178420457、化合物収率 60%

試薬・触媒・溶媒 1

HCID 8083Morpholine溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-5592581d8e494062af45e3245fc2fc98
出典データセット
uspto-grants-1978_06
特許番号
US04097479

関連ノート

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