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Ethyl Lactate → HCID 19979930, 화합물

HRID 1461500
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HRID 1461500 반응식
N(C(OCC)=O)=NC(OCC)=O.[OH:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]2[CH:25]=[CH:24][C:23]([CH:26]3[CH2:31][CH2:30][C:29]([C:40]#[N:41])([CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH3:39])[CH2:28][CH2:27]3)=[CH:22][CH:21]=2)=[CH:16][CH:15]=1.[C:42]([O:47][CH2:48][CH3:49])(=[O:46])[CH:43]([CH3:45])O>O1CCCC1>[C:40]([C:29]1([CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH3:39])[CH2:28][CH2:27][CH:26]([C:23]2[CH:24]=[CH:25][C:20]([C:17]3[CH:16]=[CH:15][C:14]([O:13][CH:43]([CH3:45])[C:42]([O:47][CH2:48][CH3:49])=[O:46])=[CH:19][CH:18]=3)=[CH:21][CH:22]=2)[CH2:31][CH2:30]1)#[N:41]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7344Ethyl LactateHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 19809977HCID 19809977, 화합물

생성물 1

HCID 19979930HCID 19979930, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

9.6 g of diethyl azodicarboxylate dissolved in tetrahydrofuran is added to a mixture of 19.4 g of 4-(4'-hydroxybiphenyl-4-yl)-1-cyano-1-octylcyclohexane, 6.5 g of ethyl lactate and 13.1 g of triphenylphosphene in 300 ml of tetrahydrofuran, stirring is carried out for one hour at 50°, the mixture is allowed to stand overnight, the solvent is removed and the residue is taken up in 100 ml of hot toluene. After the toluene solution has been cooled to 0°, it is filtered and the product is isolated from the filtrate as usual by chromatography. Optically active ethyl 2-[4'-(4-cyano-4-octylcyclohexyl)biphenyl-4-yloxy]propionate is obtained.

후처리

  1. waitto stand overnight
  2. customthe solvent is removed
  3. temperatureAfter the toluene solution has been cooled to 0°
  4. filtrationit is filtered
  5. customthe product is isolated from the filtrate as usual by chromatography

출처 및 근거

ORD 기록
ord-b36cf44ee0204a81994cf33e1d63986f
출처 데이터셋
uspto-grants-1991_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05075032

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