Acetyl chloride → Acetamide, N-(4-((1-methyl-4-phenyl-4-piperidinyl)oxy)phenyl)-

HRID 1156035

反応式

HRID 1156035 の反応式
[C:1](Cl)(=[O:3])[CH3:2].[NH2:5][C:6]1[CH:25]=[CH:24][C:9]([O:10][C:11]2([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[CH2:16][CH2:15][N:14]([CH3:17])[CH2:13][CH2:12]2)=[CH:8][CH:7]=1.C(N(CC)CC)C>C1C=CC=CC=1>[NH:5]([C:6]1[CH:25]=[CH:24][C:9]([O:10][C:11]2([C:18]3[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=3)[CH2:12][CH2:13][N:14]([CH3:17])[CH2:15][CH2:16]2)=[CH:8][CH:7]=1)[C:1]([CH3:2])=[O:3]

参加物

5

反応物 3

HCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 3060392Piperidine, 4-(p-aminophenoxy)-1-methyl-4-phenyl-

生成物 1

HCID 3060397Acetamide, N-(4-((1-methyl-4-phenyl-4-piperidinyl)oxy)phenyl)-

試薬・触媒・溶媒 1

HCID 241Benzene溶媒2 回

実験手順

A solution of 0.85 g of acetyl chloride in 5 ml of benzene is added dropwise to a solution of 2.8 g of 4-(4-aminophenoxy)-1-methyl-4-phenylpiperidine and 1.1 g of triethylamine in 10 ml of benzene. After stirring the mixture at room temperature for 6 hours, it is concentrated; the resulting residue is taken up with 30 ml each of water and diethyl ether; the obtained mixture is shaken thoroughly, and the organic phase is separated off, dried over sodium sulfate and concentrated. 2.8 g of the title compound remain as a viscous yellow oil which crystallizes (m.p. 143° to 144° C.) from diethylether after standing for several days.

後処理

  1. concentrationit is concentrated
  2. stirringthe obtained mixture is shaken thoroughly
  3. customthe organic phase is separated off
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated
  6. customcrystallizes (m.p. 143° to 144° C.) from diethylether
  7. waitafter standing for several days

出典と根拠

ORDレコード
ord-870e1b1a003c4c58bf0b300d6fd1bbc5
出典データセット
uspto-grants-1982_06
特許番号
US04333942

関連ノート

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