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Dicyclohexylcarbodiimide → HCID 178442784, 화합물

HRID 2372667
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HRID 2372667 반응식
[CH2:1]([C:11]1[CH:12]=[N:13][C:14]([C:17]2[CH:31]=[CH:30][C:20]([O:21][CH2:22][C:23]3(O)[CH2:28][CH2:27][CH2:26][CH2:25][CH2:24]3)=[CH:19][CH:18]=2)=[N:15][CH:16]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10].[F:32][C@@H:33]([CH2:37][CH2:38][CH2:39][CH3:40])[C:34]([OH:36])=[O:35].C1(N=C=NC2CCCCC2)CCCCC1>C(Cl)Cl>[F:32][C@@H:33]([CH2:37][CH2:38][CH2:39][CH3:40])[C:34]([O:36][C@H:26]1[CH2:27][CH2:28][C@H:23]([CH2:22][O:21][C:20]2[CH:30]=[CH:31][C:17]([C:14]3[N:13]=[CH:12][C:11]([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10])=[CH:16][N:15]=3)=[CH:18][CH:19]=2)[CH2:24][CH2:25]1)=[O:35]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10868DicyclohexylcarbodiimideHCID 13683897(S)-2-fluorocaproic acidHCID 86745590(p-(5-Decyl-2-pyrimidinyl)phenoxymethyl]cyclohexanol

생성물 1

HCID 178442784HCID 178442784, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

0.62 g of trans-4-[(p-(5-decyl-2-pyrimidinyl)phenoxymethyl]cyclohexanol, 0.196 g of (S)-2-fluorocaproic acid, 0.413 g of dicyclohexylcarbodiimide and 0.025 g of 4-(dimethylamino)pydidine were dissolved in 25 ml of methylene chloride and stirred at room temperature for 15 hours. The white suspension was subsequently filtered. The residue obtained after evaporation of the solvent from the filtrate was purified by chromatography on silica gel with ethyl acetate/petroleum ether (vol. 1:9). Subsequent crystallization from 10 ml of ethyl acetate and 50 ml of hexane gave 0.62 g of trans-4-[(p-(5-decyl-2-pyrimidinyl)phenoxy)methyl]cyclohexyl (S)-2-fluorohexanoate as colourless crystals, m.p. (C-S) 88.5° C., phase transitions (S-SC) 108.8° C., (SC -SA) 128° C., cl.p. (SA -I) 137.7° C.

후처리

  1. filtrationThe white suspension was subsequently filtered
  2. customThe residue obtained
  3. customafter evaporation of the solvent from the filtrate
  4. customwas purified by chromatography on silica gel with ethyl acetate/petroleum ether (vol. 1:9)
  5. customSubsequent crystallization from 10 ml of ethyl acetate and 50 ml of hexane

출처 및 근거

ORD 기록
ord-e1b5f1f87795446398a45bfddc4d5934
출처 데이터셋
uspto-grants-1992_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05100577

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