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Triphenylphosphine → HCID 19979960, 화합물

HRID 1461501
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HRID 1461501 반응식
CCOC(/N=N/C(OCC)=O)=O.[OH:13][C:14]1[CH:37]=[CH:36][C:17]([C:18]([O:20][CH:21]2[CH2:26][CH2:25][C:24]([C:34]#[N:35])([CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH3:33])[CH2:23][CH2:22]2)=[O:19])=[CH:16][CH:15]=1.C(C1(CCCCCCC)CCC(O)CC1)#N.C(OC1C=CC(C(O)=O)=CC=1)C1C=CC=CC=1.[C:71]([O:76][CH2:77][CH2:78][CH2:79][CH2:80][CH2:81][CH3:82])(=[O:75])[CH:72]([CH3:74])O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>O1CCCC1>[C:34]([C:24]1([CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH3:33])[CH2:23][CH2:22][CH:21]([O:20][C:18]([C:17]2[CH:36]=[CH:37][C:14]([O:13][CH:72]([CH3:74])[C:71]([O:76][CH2:77][CH2:78][CH2:79][CH2:80][CH2:81][CH3:82])=[O:75])=[CH:15][CH:16]=2)=[O:19])[CH2:26][CH2:25]1)#[N:35]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 6

HCID 11776TriphenylphosphineHCID 738804-(Benzyloxy)benzoic acidHCID 519757Hexyl DL-lactateHCID 5462977Diethyl azodicarboxylateHCID 19979843HCID 19979843, 화합물HCID 19979915HCID 19979915, 화합물

생성물 1

HCID 19979960
HCID 19979960, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 11.5 g of diethylazodicarboxylate in tetrahydrofuran is added to a mixture of 20.6 g of 4-cyano-4-heptylcyclohexyl p-hydroxybenzoate (obtainable by esterification of 4-cyano-4-heptylcyclohexanol with p-benzyloxybenzoic acid and cleavage of the benzyl group by catalytic hydrogenation), 11.5 g of optically active hexyl lactate and 15.7 g of triphenylphosphine in 150 ml of tetrahydrofuran, stirring is carried out for one hour at 50° and the solvent is removed after 12 hours. The residue is dissolved in 100 ml of hot toluene, cooled down, filtered and the filtrate purified as usual by chromatography and crystallization. Optically active hexyl p-(4-cyano-4-heptylcyclohexyloxycarbonyl)phenoxypropionate is obtained.

후처리

  1. customthe solvent is removed after 12 hours
  2. dissolutionThe residue is dissolved in 100 ml of hot toluene
  3. temperaturecooled down
  4. filtrationfiltered
  5. customthe filtrate purified as
  6. customusual by chromatography and crystallization

출처 및 근거

ORD 기록
ord-3184735d6ead47738da1420aa5353d4a
출처 데이터셋
uspto-grants-1991_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05075032

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