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Triphenylphosphine → HCID 22733426、化合物

HRID 2084565
ノート
印刷プレビュー

反応式

HRID 2084565 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 7

HCID 11776TriphenylphosphineHCID 650932,2'-Dipyridyl disulfideHCID 81531DiisopropylethylamineHCID 2842562Adamantan-2-ylideneacetic acidHCID 22733386HCID 22733386、化合物HCID 22733406HCID 22733406、化合物HCID 22733430HCID 22733430、化合物

生成物 1

HCID 22733426HCID 22733426、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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°).

後処理

  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

出典と根拠

ORDレコード
ord-45d29ac6cdaf45a9814c272cbec6f5c4
出典データセット
uspto-grants-2004_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06716865B1

反応ノート

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