Diisopropylethylamine → HCID 66940566、化合物

HRID 1367972ノート

反応式

HRID 1367972 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[CH:9]=[N:8][C:7]([C:15]([OH:17])=O)=[CH:6]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.[CH2:51]([O:53][C:54]([C:56]1[C:64]2[N:63]=[C:62]([NH2:65])[NH:61][C:60]=2[CH:59]=[C:58]([O:66][CH2:67][CH3:68])[CH:57]=1)=[O:55])[CH3:52]>CN(C=O)C.[Cl-].[Na+].O>[CH2:51]([O:53][C:54]([C:56]1[C:64]2[N:63]=[C:62]([NH:65][C:15]([C:7]3[N:8]=[CH:9][C:10]4[C:5]([CH:6]=3)=[CH:4][C:3]([O:2][CH3:1])=[C:12]([O:13][CH3:14])[CH:11]=4)=[O:17])[NH:61][C:60]=2[CH:59]=[C:58]([O:66][CH2:67][CH3:68])[CH:57]=1)=[O:55])[CH3:52]

参加物

7

反応物 4

HCID 81531DiisopropylethylamineHCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 14278968HCID 14278968、化合物HCID 66940226HCID 66940226、化合物

生成物 1

HCID 66940566HCID 66940566、化合物収率 63%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 57417360Sodium chloride; water溶媒

実験手順

235 mg (1.0 mmol) of 6,7-dimethoxy-isoquinoline-3-carboxylic acid and 400 mg (1.0 mmol) of HBTU were dissolved in 1.5 mL of DMF and 0.5 mL of DIEA and treated with 249 mg (1.0 mmol) of 2-amino-6-ethoxy-1H-benzoimidazole-4-carboxylic acid ethyl ester (prepared in Example 471) 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 290 mg (0.63 mmol, 63%) of 2-[(6,7-dimethoxy-isoquinoline-3-carbonyl)-amino]-6-ethoxy-1H-benzoimidazole-4-carboxylic acid ethyl ester. LCMS: 465 (M+1)+.

後処理

  1. filtrationThe resulting solid was filtered
  2. washwashed with water and EtOAc
  3. customdried under vacuum

出典と根拠

ORDレコード
ord-d65bb9384e1f401e9985f4bc2c9022f7
出典データセット
uspto-grants-2011_02
特許番号
US07893267B2

反応ノート

読み込み中…