Dicyclohexylcarbodiimide → HCID 178473054, 화합물

HRID 1683303노트

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HRID 1683303 반응식
[C:1]1([CH2:7][O:8][CH:9]([C:15]([O-:17])=O)[C:10]([O:12][CH2:13][CH3:14])=[O:11])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C1(N=C=NC2CCCCC2)CCCCC1.ON1C2C=CC=CC=2N=N1.[NH2:43][CH2:44][CH2:45][CH2:46][CH2:47][CH2:48][CH2:49][CH2:50][CH2:51][N:52]=[C:53]([NH:62][C:63](=[O:69])[O:64][C:65]([CH3:68])([CH3:67])[CH3:66])[NH:54][C:55](=[O:61])[O:56][C:57]([CH3:60])([CH3:59])[CH3:58]>ClCCl>[CH3:67][C:65]([CH3:68])([O:64][C:63]([NH:62][C:53]([NH:52][CH2:51][CH2:50][CH2:49][CH2:48][CH2:47][CH2:46][CH2:45][CH2:44][NH:43][C:15](=[O:17])[CH:9]([O:8][CH2:7][C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1)[C:10]([O:12][CH2:13][CH3:14])=[O:11])=[N:54][C:55]([O:56][C:57]([CH3:58])([CH3:59])[CH3:60])=[O:61])=[O:69])[CH3:66]

참가 물질

6

반응물 4

HCID 10868DicyclohexylcarbodiimideHCID 757711-HydroxybenzotriazoleHCID 25214054Bis(1,1-dimethylethyl) [[(8-aminooctyl)imino]methylene]biscarbamateHCID 86750947Ethyl 2-phenylmethoxypropanedioate

생성물 1

HCID 178473054HCID 178473054, 화합물수율 40.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
0 °C

실험 절차

2.6 g (10.9.10-3 mol) of ethyl 2-phenylmethoxypropanedioate are dissolved in 50 ml of dichloromethane and the mixture is cooled to 0° C. 4.34 g (22.10-3 mol) of N,N'-dicyclohexylcarbodiimide and 0.57 g (4.10-3 mol) of 1-hydroxybenzotriazole are added, the mixture is stirred for 0.5 hour, a solution of 4.21 g (10.9. 10-3 mol) of bis(1,1-dimethylethyl) [[(8-aminooctyl)imino]methylene]biscarbamate in 15 ml of dichloromethane is then added and the mixture is stirred at room temperature for 48 hours. The reaction medium is concentrated under reduced pressure and the residue is then purified by chromatography on silica using a methylcyclohexane/ethyl acetate mixture (7/3) as the eluent to give 2.7 g (yield=40.8%) of the expected product in the form of a pale yellow oil.

후처리

  1. stirringthe mixture is stirred at room temperature for 48 hours
  2. concentrationThe reaction medium is concentrated under reduced pressure
  3. customthe residue is then purified by chromatography on silica using a methylcyclohexane/ethyl acetate mixture (7/3) as the eluent

출처 및 근거

ORD 기록
ord-2ef0cf1e539e45c69803c5fb9e2aecdb
출처 데이터셋
uspto-grants-1997_06
특허 번호
US05637613

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