Triphenylphosphine → HCID 59835769, 화합물

HRID 271728

반응식

HRID 271728 반응식
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

참가 물질

6

반응물 4

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

생성물 1

HCID 59835769HCID 59835769, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ae05ed16a44b4a80af1a51e48595e914
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07452911B2

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