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

HRID 1631101ノート

反応式

HRID 1631101 の反応式
[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

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 6344Dichloromethane溶媒

実験手順

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 the course of 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 white solid; yield: 14 g of (2-amino-6-iodoquinazolin-4-yl)-(1,3-dihydroisoindol-2-yl)methanone; LC-MS retention time: 1.66 min;

後処理

  1. customthe product precipitates out as white solid

出典と根拠

ORDレコード
ord-4fff02e4bc614ef6b5e63ada9fa71a78
出典データセット
uspto-grants-2014_07
特許番号
US08791129B2

反応ノート

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