Phenethyl bromide → HCID 6483409、化合物

HRID 2227466ノート

反応式

HRID 2227466 の反応式
[CH3:1][S:2][C:3]1[C:7]([C:8]#[N:9])=[C:6]([C:10]2[CH:15]=[CH:14][C:13]([OH:16])=[CH:12][CH:11]=2)[O:5][N:4]=1.[C:17]1([CH2:23][CH2:24]Br)[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.C([O-])([O-])=O.[K+].[K+]>CC(C)=O>[CH3:1][S:2][C:3]1[C:7]([C:8]#[N:9])=[C:6]([C:10]2[CH:15]=[CH:14][C:13]([O:16][CH2:24][CH2:23][C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)=[CH:12][CH:11]=2)[O:5][N:4]=1

参加物

5

反応物 3

HCID 7666Phenethyl bromideHCID 11430Potassium CarbonateHCID 135525222HCID 135525222、化合物

生成物 1

HCID 6483409HCID 6483409、化合物収率 80%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

Equimolecular amounts of (III), 2-phenyl-ethyl bromide and K2CO3 were refluxed in acetone for 48 h. The mixture was concentrated to small volume and shaken with diethyl ether and water. The ether phase was washed with 2 M NaOH, then with water, evaporated to dryness and the residue was recrystallized from ethanol. The title product was obtained in an 80% yield (abbreviation ON-6), m.p. 93-940° C. (ethanol); IR (KBr) 2227 (CN) cm1; 1H NMR (CDCl3) (δ, ppm) 2.66 (s, 3H, SCH3); 3.14 (t, 2H, CH2—Ph); 4.26 (t, 2H, O—CH2); 7.30 (m, 5H, arom.); 6.99-8.00 (m, 4H, arom.).

後処理

  1. concentrationThe mixture was concentrated to small volume
  2. washThe ether phase was washed with 2 M NaOH
  3. customwith water, evaporated to dryness
  4. customthe residue was recrystallized from ethanol

出典と根拠

ORDレコード
ord-256d619071ed4830aebb4e85f484e208
出典データセット
uspto-grants-2002_07
特許番号
US06414004B1

反応ノート

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