Hexamethylenetetramine → HCID 20337667、化合物

HRID 1395621ノート

反応式

HRID 1395621 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-one2 回

生成物 1

HCID 20337667HCID 20337667、化合物収率 95%

実験手順

88 g of p-tetradecyloxy-ω-bromoacetophenone (stage 2 of compound 29) are dissolved in 320 ml of dried chloroform. 30.4 g of urotropin are added at room temperature. The solution undergoes spontaneous heating. It is stirred for 2 hours at room temperature. The chloroform is distilled off and the solid residue is rubbed with acetone. The crystalline deposit is filtered off under suction and washed repeatedly with acetone. The crude product is then introduced into a solution of 140 ml of concentrated sulphuric acid in 100 ml of ethanol, followed by stirring for 24 hours at room temperature. After filtration under suction, the residue is washed with a mixture of ethanol and concentrated hydrochloric acid (7:1), giving 80 g=95% of p-tetradecyloxy-ω-aminoacetophenone hydrochloride melting at 190°-195° C.

後処理

  1. distillationThe chloroform is distilled off
  2. filtrationThe crystalline deposit is filtered off under suction
  3. washwashed repeatedly with acetone
  4. additionThe crude product is then introduced into a solution of 140 ml of concentrated sulphuric acid in 100 ml of ethanol
  5. stirringby stirring for 24 hours at room temperature
  6. filtrationAfter filtration under suction
  7. washthe residue is washed with a mixture of ethanol and concentrated hydrochloric acid (7:1)

出典と根拠

ORDレコード
ord-576c2a364c9a4e2291a8bfab5ab912e4
出典データセット
uspto-grants-1980_05
特許番号
US04204867

反応ノート

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