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Dicyclohexylcarbodiimide → HCID 21649526, 화합물

HRID 846565
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HRID 846565 반응식
C(OC(C1C=CC(C(O)=O)=CC=1)=O)CCCCCCC.O[C:22]1[CH:27]=[CH:26][C:25]([C:28]2[CH:33]=[CH:32][C:31]([C:34](=[O:43])[CH:35]([CH3:42])[CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH3:41])=[CH:30][CH:29]=2)=[CH:24][CH:23]=1.C1(N=C=NC2CCCCC2)CCCCC1>CN(C)C1C=CN=CC=1.C(Cl)Cl>[CH3:42][CH:35]([CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH3:41])[C:34]([C:31]1[CH:32]=[CH:33][C:28]([C:25]2[CH:26]=[CH:27][CH:22]=[CH:23][CH:24]=2)=[CH:29][CH:30]=1)=[O:43]
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참가 물질

6

반응물 3

HCID 10868DicyclohexylcarbodiimideHCID 145974864-Hydroxy-4'-(2-methyloctanoyl) biphenylHCID 20143990HCID 20143990, 화합물

생성물 1

HCID 21649526HCID 21649526, 화합물수율 46%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344
Dichloromethane
용매

실험 절차

To 10 ml of methylene chloride were added 85 mg (0.31 mmol) of 4-octyloxycarbonyl benzoic acid obtained in Example 32, 95 mg (0.31 mmol) of 4-hydroxy-4'-(2-methyloctanoyl) biphenyl and 20 mg of 4-dimethylamino pyridine, which was added with 70 mg (0.32 mmol) of N,N'-dicyclohexylcarbodiimide. This mixture was reacted by heating under reflux for 4 hours, and the precipitated solid was filtered off. The filtrate was concentrated and isolated by a column chromatography of silica gel to obtain 42 mg (yield 24%) of white (+)-4-(2-methyloctanoyl) biphenyl, 4-octyloxycarbonyl benzoic acid ester having the aforementioned physical and chemical properties.

후처리

  1. customThis mixture was reacted
  2. temperatureby heating
  3. temperatureunder reflux for 4 hours
  4. filtrationthe precipitated solid was filtered off
  5. concentrationThe filtrate was concentrated
  6. customisolated by a column chromatography of silica gel

출처 및 근거

ORD 기록
ord-1d3b3692813a411f80c36559a253cc29
출처 데이터셋
uspto-grants-1992_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05137653

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