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Diisopropylamine → HCID 23370104, 화합물

HRID 1901049
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HRID 1901049 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH:8][C:9](=[O:25])[C:10]1[CH:15]=[C:14]([C:16]([CH3:19])([CH3:18])[CH3:17])[C:13]([OH:20])=[C:12]([C:21]([CH3:24])([CH3:23])[CH3:22])[CH:11]=1.C(NC(C)C)(C)C.Cl[C:34]([O:36][C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1)=[O:35]>ClCCl>[C:21]([C:12]1[CH:11]=[C:10]([CH:15]=[C:14]([C:16]([CH3:18])([CH3:19])[CH3:17])[C:13]=1[OH:20])[C:9]([NH:8][C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=1[NH:1][C:34](=[O:35])[O:36][C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1)=[O:25])([CH3:24])([CH3:23])[CH3:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7912DiisopropylamineHCID 15891Phenyl chloroformateHCID 23370116N-(2-aminophenyl)-3,5-di-t-butyl-4-hydroxybenzamide

생성물 1

HCID 23370104HCID 23370104, 화합물수율 1,095.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

N-(2-aminophenyl)-3,5-di-t-butyl-4-hydroxybenzamide (0.85 g) and diisopropylamine (0.39 ml) were suspended in dichloromethane (20 ml) and a solution of phenyl chloroformate (16.8 g) in dichloromethane (30 ml) was added dropwise under ice-cooling. After stirring the mixture overnight, the reaction solution was washed with water, saturated saline, dried over anhydrous MgSO4 and the solvent was distilled off. Purification of the residue by a silica gel column chromatography (chloroform:ethyl acetate=10:1) followed by crystallization from hexane/ethyl acetate afforded phenyl N-[2-(3,5-di-t-butyl-4-hydroxybenzoylamino)phenyl]carbamate (12.6 g, 49%).

후처리

  1. temperaturecooling
  2. washthe reaction solution was washed with water, saturated saline
  3. dry with materialdried over anhydrous MgSO4
  4. distillationthe solvent was distilled off
  5. customPurification of the residue by a silica gel column chromatography (chloroform:ethyl acetate=10:1)
  6. customfollowed by crystallization from hexane/ethyl acetate

출처 및 근거

ORD 기록
ord-4e8c09844fd24b25af4c01a57dab1cc3
출처 데이터셋
uspto-grants-1996_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05576335

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