Sulfuric Acid → HCID 13281039, 화합물

HRID 648652노트

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HRID 648652 반응식
[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

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 11989373ethyl 4-(cyanomethyl)benzoateHCID 54128206HCID 54128206, 화합물

생성물 1

HCID 13281039HCID 13281039, 화합물

시약·촉매·용매 1

HCID 72391,2-Dichlorobenzene용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c2372fe392ae404f83039c363e8b0916
출처 데이터셋
uspto-grants-1988_04
특허 번호
US04735959

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