Crotononitrile → Evandamine

HRID 745758ノート

反応式

HRID 745758 の反応式
Cl.[NH:2]([C:4]1[S:5][C:6]2[CH2:12][CH2:11][CH2:10][CH2:9][C:7]=2[N:8]=1)[NH2:3].CC[O-].[Na+].[Na].[C:18](#[N:22])/[CH:19]=[CH:20]/[CH3:21]>O.C(O)C>[NH2:22][C:18]1[CH2:19][CH:20]([CH3:21])[N:2]([C:4]2[S:5][C:6]3[CH2:12][CH2:11][CH2:10][CH2:9][C:7]=3[N:8]=2)[N:3]=1

参加物

7

反応物 4

HCID 637921CrotononitrileHCID 2723922Sodium ethoxideHCID 5360545SodiumHCID 23312423HCID 23312423、化合物

生成物 1

HCID 3038554Evandamine収率 60.9%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒2 回HCID 962Water溶媒

実験手順

20 g of 2-hydrazino-4,5,6,7-tetrahyro-benzothiazole hydrochloride are added to a sodium ethylate solution of 5.7 g of sodium and 250 ml of ethanol and the mixture is stirred at room temperature for 10 minutes. 5.5 g of crotononitrile are then added dropwise and the mixture is boiled under reflux for 5 hours. After cooling, the ethanol is stripped off in vacuo and the residue is taken up in water. The insoluble material is filtered off and washed thoroughly with water, acetone and ether in succession. After drying, 11.8 g of beige crystals of 3-amino-5-methyl-1-(4,5,6,7-tetrahydro-benzothiazolyl)-2-pyrazoline of melting point 247°-249° C. are obtained.

後処理

  1. temperatureunder reflux for 5 hours
  2. temperatureAfter cooling
  3. filtrationThe insoluble material is filtered off
  4. washwashed thoroughly with water, acetone and ether in succession
  5. customAfter drying

出典と根拠

ORDレコード
ord-49c689f31b734893be0dda0216d25fa6
出典データセット
uspto-grants-1986_07
特許番号
US04600722

反応ノート

読み込み中…