Triphenylphosphine → HCID 69384193、化合物

HRID 916830ノート

反応式

HRID 916830 の反応式
[CH3:1][C:2]1([CH3:27])[O:7][C:6]2[CH:8]=[CH:9][C:10]([C@H:12]3[O:16][C:15](=[O:17])[N:14]([CH2:18][CH2:19][C:20]4[CH:25]=[CH:24][C:23]([OH:26])=[CH:22][CH:21]=4)[CH2:13]3)=[CH:11][C:5]=2[CH2:4][O:3]1.O[CH2:29][CH2:30][O:31][CH2:32][C:33]1[CH:34]=[C:35]([CH:40]=[CH:41][CH:42]=1)[C:36]([O:38][CH3:39])=[O:37].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(N1CCCCC1)=O)=NC(N1CCCCC1)=O>C(Cl)Cl>[CH3:1][C:2]1([CH3:27])[O:7][C:6]2[CH:8]=[CH:9][C:10]([C@H:12]3[O:16][C:15](=[O:17])[N:14]([CH2:18][CH2:19][C:20]4[CH:21]=[CH:22][C:23]([O:26][CH2:29][CH2:30][O:31][CH2:32][C:33]5[CH:34]=[C:35]([CH:40]=[CH:41][CH:42]=5)[C:36]([O:38][CH3:39])=[O:37])=[CH:24][CH:25]=4)[CH2:13]3)=[CH:11][C:5]=2[CH2:4][O:3]1

参加物

6

反応物 4

HCID 11776TriphenylphosphineHCID 730421,1'-(Azodicarbonyl)dipiperidineHCID 23344098HCID 23344098、化合物HCID 69384373HCID 69384373、化合物

生成物 1

HCID 69384193HCID 69384193、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

(5R)-5(2,2-Dimethyl-4H-1,3-benzodioxin-6-yl)-3-[2-(4-hydroxyphenyl)ethyl]-1,3-oxazolidin-2-one{Example 28 v)} (300 mg), methyl 3-[(2-hydroxyethoxy)methyl]benzoate (340 mg) and triphenylphosphine (642 mg) were dissolved in DCM (10 ml) and stirred for 15 min. To this was added 1,1′-(azodicarbonyl)dipiperidine (612 mg) and the solution was stirred for 16 h. The solution was then diluted in DCM, washed with water, dried (MgSO4) and concentrated in vacuo. The residue was purified by chromatography (Biotage, 90 g) eluting with CH2Cl2-MeOH (250:1) to give the title compound (450 mg). LCMS RT=3.62 min.

後処理

  1. stirringthe solution was stirred for 16 h
  2. washwashed with water
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by chromatography (Biotage, 90 g)
  6. washeluting with CH2Cl2-MeOH (250:1)

出典と根拠

ORDレコード
ord-8f071fd45c3442bd868834ff2eea922a
出典データセット
uspto-grants-2007_09
特許番号
US07271197B2

反応ノート

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