Dicyclohexylcarbodiimide → HCID 178473054、化合物

HRID 1683303ノート

反応式

HRID 1683303 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 178473054HCID 178473054、化合物収率 40.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2ef0cf1e539e45c69803c5fb9e2aecdb
出典データセット
uspto-grants-1997_06
特許番号
US05637613

反応ノート

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