Diisopropylethylamine → isoquinoline-3-carboxylic acid [5-ethylsulfanyl-7-(1H-imidazol-2-ylcarbamoyl)-1H-benzoimidazol-2-yl]-amide

HRID 1367996

反応式

[CH2:1]([S:3][C:4]1[CH:5]=[C:6]([C:26]([OH:28])=O)[C:7]2[NH:11][C:10]([NH:12][C:13]([C:15]3[N:16]=[CH:17][C:18]4[C:23]([CH:24]=3)=[CH:22][CH:21]=[CH:20][CH:19]=4)=[O:14])=[N:9][C:8]=2[CH:25]=1)[CH3:2].CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C.S(O)(O)(=O)=O.[NH2:67][C:68]1[NH:69][CH:70]=[CH:71][N:72]=1>CN(C=O)C.[Cl-].[Na+].O>[CH2:1]([S:3][C:4]1[CH:5]=[C:6]([C:26](=[O:28])[NH:67][C:68]2[NH:69][CH:70]=[CH:71][N:72]=2)[C:7]2[NH:11][C:10]([NH:12][C:13]([C:15]3[N:16]=[CH:17][C:18]4[C:23]([CH:24]=3)=[CH:22][CH:21]=[CH:20][CH:19]=4)=[O:14])=[N:9][C:8]=2[CH:25]=1)[CH3:2]

参加物

実験手順

80 mg (0.2 mmol) of 6-ethylsulfanyl-2-[(isoquinoline-3-carbonyl)-amino]-3H-benzoimidazole-4-carboxylic acid and 300 mg (0.76 mmol) of HBTU were dissolved in 1.0 mL of DMF and 0.5 mL of DIEA and treated with 132 mg (1.0 mmol) of 2-aminoimidazole sulfate as described in general procedure A. Upon completion, the reaction was diluted with brine. The resulting solid was filtered, washed with water and EtOAc, and dried under vacuum to produce 66 mg (71%) of isoquinoline-3-carboxylic acid [5-ethylsulfanyl-7-(1H-imidazol-2-ylcarbamoyl)-1H-benzoimidazol-2-yl]-amide. LCMS: 458 (M+1)+.

後処理

filtrationThe resulting solid was filtered
washwashed with water and EtOAc
customdried under vacuum

出典と根拠

ORDレコード: ord-009aa793948a4e398d05a3504f0ac1f4
出典データセット: uspto-grants-2011_02
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US07893267B2

反応式

参加物

反応物 4

生成物 1

試薬・触媒・溶媒 2

実験手順

後処理

出典と根拠

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