Sulfuric Acid → HCID 13281039、化合物

HRID 648652ノート

反応式

HRID 648652 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([CH:8](O)[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[N:15]2[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]2)[CH:5]=[CH:6][CH:7]=1.[C:22]([CH2:24][C:25]1[CH:35]=[CH:34][C:28]([C:29]([O:31][CH2:32][CH3:33])=[O:30])=[CH:27][CH:26]=1)#[N:23].S(=O)(=O)(O)[OH:37]>ClC1C=CC=CC=1Cl>[CH3:1][C:2]1[CH:3]=[C:4]([CH:8]([NH:23][C:22]([CH2:24][C:25]2[CH:35]=[CH:34][C:28]([C:29]([O:31][CH2:32][CH3:33])=[O:30])=[CH:27][CH:26]=2)=[O:37])[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[N:15]2[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]2)[CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 11989373ethyl 4-(cyanomethyl)benzoateHCID 54128206HCID 54128206、化合物

生成物 1

HCID 13281039HCID 13281039、化合物

試薬・触媒・溶媒 1

HCID 72391,2-Dichlorobenzene溶媒2 回

実験手順

A mixture of 0.22 gm (0.8 m mol) of α-(3-methyl-phenyl)-2-piperidino-benzyl alcohol and 0.15 gm (0.8 m mol) of ethyl 4-cyanomethyl-benzoate in 2 ml of o-dichlorobenzene was added dropwise, at ambient temperature, to 1.5 ml of o-dichlorobenzene and 1.5 ml of concentrated sulfuric acid. After stirring for two hours, the mixture was poured onto ice water, extracted once with ether, made alkaline with dilute sodium hydroxide solution, and extracted with chloroform. The chloroform extract was concentrated by evaporation, and the residue was recrystallized from ethanol.

後処理

  1. additionthe mixture was poured onto ice water
  2. extractionextracted once with ether
  3. extractionextracted with chloroform
  4. extractionThe chloroform extract
  5. concentrationwas concentrated by evaporation
  6. customthe residue was recrystallized from ethanol

出典と根拠

ORDレコード
ord-c2372fe392ae404f83039c363e8b0916
出典データセット
uspto-grants-1988_04
特許番号
US04735959

反応ノート

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