Dichloromethane → HCID 68058495, 화합물

HRID 1186818노트

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HRID 1186818 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[C:13]3=[N:14][CH:15]=[CH:16][C:17](I)=[C:12]3[CH:11]=[N:10]2)[CH:5]=[C:6]([F:8])[CH:7]=1.CC1(C)C(C)(C)[O:23][B:22](B2OC(C)(C)C(C)(C)O2)[O:21]1.C([O-])(=O)C.[K+].C(Cl)Cl>CS(C)=O>[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[C:13]3=[N:14][CH:15]=[CH:16][C:17]([B:22]([OH:23])[OH:21])=[C:12]3[CH:11]=[N:10]2)[CH:5]=[C:6]([F:8])[CH:7]=1

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 517044Potassium AcetateHCID 2733548Bis(pinacolato)diboraneHCID 68058174HCID 68058174, 화합물

생성물 1

HCID 68058495HCID 68058495, 화합물

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

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온도
85 °C

실험 절차

To a 48 mL pressure bottle containing Intermediate 75A (558.6 mg, 1.46 mmol) was added 4,4,4′,4′,5,5,5′,5′-octamethyl-2,2′-bi(1,3,2-dioxaborolane) (569.2 mg, 2.24 mmol), potassium acetate (584.3 mg, 5.95 mmol), and anhydrous DMSO (11 mL). The reaction mixture was flushed with argon and treated with PdCl2(dppf).CH2Cl2 (59.1 mg, 0.081 mmol). The reaction mixture was heated to 85° C. for 1 h and then at 105° C. for 1.5 h to give conversion to the desired product. LC/MS (Condition B): ret. T=4.29 min, (M+H)+ 291.99, 292.99.

후처리

  1. customThe reaction mixture was flushed with argon
  2. additiontreated with PdCl2(dppf)

출처 및 근거

ORD 기록
ord-bf43cf5635e94e5fb9dceec48f5abb6a
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08673922B2

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