Hexamethylenetetramine → HCID 20337667、化合物

HRID 2052195ノート

反応式

HRID 2052195 の反応式
[CH2:1]([O:15][C:16]1[CH:21]=[CH:20][C:19]([C:22](=[O:25])[CH2:23]Br)=[CH:18][CH:17]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14].C1N2CN3CN(C2)C[N:27]1C3.C(Cl)(Cl)[Cl:37]>>[ClH:37].[CH2:1]([O:15][C:16]1[CH:21]=[CH:20][C:19]([C:22](=[O:25])[CH2:23][NH2:27])=[CH:18][CH:17]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14]

参加物

4

反応物 3

HCID 4101HexamethylenetetramineHCID 6212ChloroformHCID 539946982-Bromo-1-[4-(tetradecyloxy)phenyl]ethan-1-one

生成物 1

HCID 20337667HCID 20337667、化合物収率 95%

実験手順

88 g of p-tetradecyloxy-ω-bromoacetophenone are dissolved in 320 ml of anhydrous chloroform. 30.4 g of urotropine are added at room temperature. The solution heats up spontaneously. It is then stirred for 2 hours at room temperature. The chloroform is evaporated off and the solid residue is triturated with acetone. The crystalline precipitate is suction filtered and washed several times with acetone. The crude product is then introduced into a solution of 140 ml of concentrated hydrochloric acid in 1000 ml of ethanol and stirred for 24 hours at room temperature. The product is suction filtered and washed with a mixture of ethanol and concentrated hydrochloric acid (7:1). 80 g =95% of p-tetradecyloxy-ω-aminoacetophenone-hydrochloride melting at 190° to 195° C. are obtained.

後処理

  1. customThe chloroform is evaporated off
  2. customthe solid residue is triturated with acetone
  3. filtrationfiltered
  4. washwashed several times with acetone
  5. additionThe crude product is then introduced into a solution of 140 ml of concentrated hydrochloric acid in 1000 ml of ethanol
  6. stirringstirred for 24 hours at room temperature
  7. filtrationfiltered
  8. washwashed with a mixture of ethanol and concentrated hydrochloric acid (7:1)

出典と根拠

ORDレコード
ord-26dcca492c964e50af4a71761917c409
出典データセット
uspto-grants-1980_01
特許番号
US04183752

反応ノート

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