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Triphenylphosphine → HCID 22733426, 화합물

HRID 2084565
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HRID 2084565 반응식
[CH:1]12[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]3)[C:2]1=[CH:11][C:12]([NH:14][C:15]1[CH:20]=[CH:19][C:18]([OH:21])=[CH:17][C:16]=1O)=O)[CH2:8]2.C12(CC(NC3C=CC(O)=CC=3O)=O)CC3CC(CC(C3)C1)C2.C12CC3CC(CC(C3)C1=CC(O)=O)C2.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N1C=CC=CC=1[S:84]SC1C=CC=CN=1.C(N(C(C)C)C(C)C)C.[OH-].OC1C=C(O)C=CC=1N>ClCCl>[CH:1]12[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]3)[C:2]1=[CH:11][C:12]1[S:84][C:16]3[CH:17]=[C:18]([OH:21])[CH:19]=[CH:20][C:15]=3[N:14]=1)[CH2:8]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 7

HCID 11776TriphenylphosphineHCID 650932,2'-Dipyridyl disulfideHCID 81531DiisopropylethylamineHCID 2842562Adamantan-2-ylideneacetic acidHCID 22733386HCID 22733386, 화합물HCID 22733406HCID 22733406, 화합물HCID 22733430HCID 22733430, 화합물

생성물 1

HCID 22733426HCID 22733426, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2-(Adamantan-2-ylidene)-N-(2,4-dihydroxyphenyl)acetamide (formula VII) 3.0 g (adamantan-2-ylidene)acetic acid (formula R3COOH), 5.91 g triphenylphosphane and 4.95 g dipyridyldisulfide, dissolved in 100 ml of dichloromethane, are stirred at room temperature overnight. To the mixture obtained, 5.13 ml of N-ethyl-diisopropylamine and 4.83 g 2,4-dihydroxyaniline hydroxide (formula V) are added and the mixture is stirred for about 24 hours, the solvent is evaporated off, the evaporation residue is dissolved in ethyl acetate and extracted with a saturated aqueous NaH2PO4 solution and brine. The organic layer is dried, the solvent is evaporated off and the residue is purified by chromatography. The title compound is obtained (m.p. 166-169°).

후처리

  1. customTo the mixture obtained
  2. stirringthe mixture is stirred for about 24 hours
  3. customthe solvent is evaporated off
  4. dissolutionthe evaporation residue is dissolved in ethyl acetate
  5. extractionextracted with a saturated aqueous NaH2PO4 solution and brine
  6. customThe organic layer is dried
  7. customthe solvent is evaporated off
  8. customthe residue is purified by chromatography

출처 및 근거

ORD 기록
ord-45d29ac6cdaf45a9814c272cbec6f5c4
출처 데이터셋
uspto-grants-2004_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06716865B1

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