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Diethyl phthalimidomalonate → HCID 10875852, 화합물

HRID 581392
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HRID 581392 반응식
[C:1]1(=[O:22])[N:5]([CH:6]([C:12]([O:14]CC)=O)[C:7]([O:9][CH2:10][CH3:11])=[O:8])[C:4](=[O:17])[C:3]2=[CH:18][CH:19]=[CH:20][CH:21]=[C:2]12.[Cl:23][C:24]1[CH:30]=[C:29]([S:31]([CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH3:45])(=[O:33])=[O:32])[CH:28]=[CH:27][C:25]=1[NH2:26]>C1(C)C(C)=CC=CC=1>[Cl:23][C:24]1[CH:30]=[C:29]([S:31]([CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH3:45])(=[O:32])=[O:33])[CH:28]=[CH:27][C:25]=1[NH:26][C:12](=[O:14])[CH:6]([N:5]1[C:4](=[O:17])[C:3]2=[CH:18][CH:19]=[CH:20][CH:21]=[C:2]2[C:1]1=[O:22])[C:7]([O:9][CH2:10][CH3:11])=[O:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 79760Diethyl phthalimidomalonateHCID 108613032-Chloro-4-dodecylsulfonylaniline

생성물 1

HCID 10875852HCID 10875852, 화합물

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

Diethyl 2-phthalimidomalonate (obtained from Aldrich Chemical Company Limited) (9.8 g, 32.0 mmol) and 2-chloro-4-dodecylsulphonylaniline (11.5 g, 32.0 mmol) were added to xylene (250 ml) and refluxed under a Dean and Stark trap for 96 hr. The distillate was periodically removed and the main bulk of solvent replenished as necessary. Removal of the xylene solvent under reduced pressure afforded a light brown oil which was purified by column chromatography using a 4:1 mixture of 60-80° C. petroleum ether:ethyl acetate and silica gel. The product, coupler (C13), was obtained as a white solid which was slurried with a little petroleum ether, filtered and dried in air, 13.6 g, 67%.

후처리

  1. temperaturerefluxed under a Dean and Stark trap for 96 hr
  2. customThe distillate was periodically removed
  3. customRemoval of the xylene solvent under reduced pressure
  4. customafforded a light brown oil which
  5. customwas purified by column chromatography
  6. additiona 4:1 mixture of 60-80° C. petroleum ether
  7. customThe product, coupler (C13), was obtained as a white solid which
  8. filtrationfiltered
  9. customdried in air, 13.6 g, 67%

출처 및 근거

ORD 기록
ord-fac4538d97994630a882626d791dd64f
출처 데이터셋
uspto-grants-1999_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05919969

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