Triphenylphosphine → HCID 59835746、化合物

HRID 1916722

反応式

HRID 1916722 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][CH2:35][OH:36])=[N:31][CH:32]=2)=[CH:23][CH:22]=1.[N:37]1([CH2:42][C:43]2[CH:48]=[CH:47][C:46](O)=[CH:45][CH:44]=2)[CH2:41][CH2:40][CH2:39][CH2:38]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][CH2:35][O:36][C:46]3[CH:45]=[CH:44][C:43]([CH2:42][N:37]4[CH2:41][CH2:40][CH2:39][CH2:38]4)=[CH:48][CH:47]=3)=[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 690763373-[5-(4-Chloro-phenyl)-pyridin-2-yl]-prop-2-yn-1-ol

生成物 1

HCID 59835746HCID 59835746、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 100 mg (0.41 mmol) 3-[5-(4-chloro-phenyl)-pyridin-2-yl]-prop-2-yn-1-ol and 88 mg (0.5 mmol) 4-pyrrolidin-1-ylmethyl-phenol in 4 mL THF. Then 0.1 mL (0.5 mmol) diisopropyl azo-dicarboxylate is slowly added dropwise and the reaction mixture is stirred for 3 h at RT. The mixture is evaporated down i. vac., the residue is taken up in 1 mL DMF and purified by HPLC. The product obtained, which still contains triphenylphosphane oxide, is again purified by chromatography (silica gel, EtOAc after EtOAc/MeOH/NH3 9:1:0.1).

後処理

  1. customThe mixture is evaporated down i
  2. custompurified by HPLC
  3. customThe product obtained
  4. customwhich still contains triphenylphosphane oxide, is again purified by chromatography (silica gel, EtOAc after EtOAc/MeOH/NH3 9:1:0.1)

出典と根拠

ORDレコード
ord-f08aa4f833cf41098db3611a2b4d8708
出典データセット
uspto-grants-2013_12
特許番号
US08618132B2

関連ノート

読み込み中…