Potassium Carbonate → HCID 14074168、化合物

HRID 620042

反応式

HRID 620042 の反応式
Br.Br.[OH:3][C:4]1[CH:9]=[CH:8][C:7]([N:10]2[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]2)=[CH:6][CH:5]=1.Cl[C:17]1[O:18][C:19]2[CH:25]=[CH:24][CH:23]=[CH:22][C:20]=2[N:21]=1.C([O-])([O-])=O.[K+].[K+]>CN(C)C=O>[OH:3][C:4]1[CH:5]=[CH:6][C:7]([N:10]2[CH2:15][CH2:14][N:13]([C:17]3[O:18][C:19]4[CH:25]=[CH:24][CH:23]=[CH:22][C:20]=4[N:21]=3)[CH2:12][CH2:11]2)=[CH:8][CH:9]=1

参加物

5

反応物 3

HCID 11430Potassium Carbonate3 回HCID 119862-ChlorobenzoxazoleHCID 2723591p-(1-Piperazinyl)phenol dihydrobromide

生成物 1

HCID 14074168HCID 14074168、化合物収率 97.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
85 °C

実験手順

A mixture of 5.11 g (15 mmol) of 1-(4-hydroxyphenyl)piperazine dihydrobromide, 2.46 g (16 mmol) of 2-chlorobenzoxazole and 2.18 g (15.8 mmol) of powdered K2CO3 in 55 ml of absolute N,N-dimethylformamide was warmed to 85° C., and 345 mg of powdered K2CO3 were added with stirring under a nitrogen atmosphere in each case after 10 minutes, after a further 25 minutes and after a further 60 minutes (total addition of 1.035 g (7.5 mmol) of K2CO3). The mixture was stirred for a further 3 hours at 85° C., the DMF was substantially removed by distillation in an oil-pump vacuum in a rotary evaporator, the crystalline residue was mixed with 50 ml of water, and this mixture was shaken for 15 minutes. The mixture was then filtered under suction and the filter residue was washed with water and dried in vacuo. 4.30 g (97% of theory) of pure 1-(4-hydroxyphenyl)-4-(benzoxazol-2-yl)piperazine, melting point 161°-3° C., were obtained,

後処理

  1. stirringThe mixture was stirred for a further 3 hours at 85° C.
  2. customthe DMF was substantially removed by distillation in an oil-pump vacuum in a rotary evaporator
  3. additionthe crystalline residue was mixed with 50 ml of water
  4. stirringthis mixture was shaken for 15 minutes
  5. filtrationThe mixture was then filtered under suction
  6. washthe filter residue was washed with water
  7. customdried in vacuo

出典と根拠

ORDレコード
ord-3f4b8fdb47f94dfdab03d170978fb3fe
出典データセット
uspto-grants-1989_04
特許番号
US04818758

関連ノート

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