Triphenylphosphine → HCID 59835769、化合物

HRID 271728

反応式

HRID 271728 の反応式
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Cl:20][C:21]1[CH:26]=[CH:25][C:24]([C:27]2[CH:28]=[CH:29][C:30]([C:33]#[C:34][C:35]([CH3:38])([OH:37])[CH3:36])=[N:31][CH:32]=2)=[CH:23][CH:22]=1.[N:39]1([CH2:44][C:45]2[CH:50]=[CH:49][C:48](O)=[CH:47][CH:46]=2)[CH2:43][CH2:42][CH2:41][CH2:40]1.N(C(OC(C)C)=O)=NC(OC(C)C)=O>C1COCC1>[Cl:20][C:21]1[CH:26]=[CH:25][C:24]([C:27]2[CH:28]=[CH:29][C:30]([C:33]#[C:34][C:35]([CH3:38])([O:37][C:48]3[CH:47]=[CH:46][C:45]([CH2:44][N:39]4[CH2:43][CH2:42][CH2:41][CH2:40]4)=[CH:50][CH:49]=3)[CH3:36])=[N:31][CH:32]=2)=[CH:23][CH:22]=1

参加物

6

反応物 4

HCID 11776TriphenylphosphineHCID 75555Diisopropyl diazene-1,2-dicarboxylateHCID 187719784-(Pyrrolidin-1-ylmethyl)phenolHCID 69077452HCID 69077452、化合物

生成物 1

HCID 59835769HCID 59835769、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

131 mg (0.5 mmol) triphenylphosphane are added to a solution of 136 mg (0.5 mmol) 4-[5-(4-chloro-phenyl)-pyridin-2-yl]-2-methyl-but-3-yn-2-ol and 88 mg (0.5 mmol) 4-pyrrolidin-1-ylmethyl-phenol in 20 ml THF. Then 0.1 mL (0.5 mmol) diisopropyl azo-dicarboxylate is slowly added dropwise and the reaction mixture is stirred for 24 h at RT. The mixture is evaporated down i.vac., the residue is taken up in water, extracted exhaustively with EtOAc, the organic phase is washed with saturated NaCl solution and dried over Na2SO4. After the desiccant and solvent have been eliminated the residue is purified by HPLC.

後処理

  1. customThe mixture is evaporated down i.vac
  2. extractionextracted exhaustively with EtOAc
  3. washthe organic phase is washed with saturated NaCl solution
  4. dry with materialdried over Na2SO4
  5. customis purified by HPLC

出典と根拠

ORDレコード
ord-ae05ed16a44b4a80af1a51e48595e914
出典データセット
uspto-grants-2008_11
特許番号
US07452911B2

関連ノート

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