Hydrochloric Acid → (2-Amino-6-iodoquinazolin-4-yl)isoindolin-2-ylmethanone

HRID 1037679노트

반응식

HRID 1037679 반응식
[CH2:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH2:3][N:2]1[C:10](=[O:28])[C:11]([C:13]1[CH:18]=[C:17]([I:19])[CH:16]=[CH:15][C:14]=1[NH:20]C(=O)OC(C)(C)C)=O.[F-].[Cs+].C[Si]([N:35]=[C:36]=[N:37][Si](C)(C)C)(C)C.Cl>C(#N)C.ClCCl>[NH2:35][C:36]1[N:37]=[C:11]([C:10]([N:2]2[CH2:3][C:4]3[C:9](=[CH:8][CH:7]=[CH:6][CH:5]=3)[CH2:1]2)=[O:28])[C:13]2[C:14](=[CH:15][CH:16]=[C:17]([I:19])[CH:18]=2)[N:20]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 25953Cesium fluorideHCID 70473Bis(trimethylsilyl)carbodiimideHCID 59483457Tert-butyl {2-[2-(1,3-dihydroisoindol-2-yl)-2-oxoacetyl]-4-iodophenyl}carbamate

생성물 1

HCID 58457195(2-Amino-6-iodoquinazolin-4-yl)isoindolin-2-ylmethanone

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 6344Dichloromethane용매

실험 절차

24.50 g of tert-butyl {2-[2-(1,3-dihydroisoindol-2-yl)-2-oxoacetyl]-4-iodophenyl}carbamate are dissolved in 500 ml of acetonitrile under argon. 0.756 g of caesium fluoride is added, and 16.887 ml of bis(trimethylsilyl)-carbodiimide are added dropwise to the solution over 5 min. The mixture is stirred at room temperature for 15 min, and 400 ml of dichloromethane are added. After addition of 400 ml of hydrochloric acid (1N), the product precipitates out as a white solid. Yield: 14 g of (2-amino-6-iodoquinazolin-4-yl)-(1,3-dihydroisoindol-2-yl)methanone; LC-MS retention time: 1.655 min;

후처리

  1. customthe product precipitates out as a white solid

출처 및 근거

ORD 기록
ord-4aa3e74dd777475db83a4de2f95cb280
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08546565B2

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