Methanol → 3-Benzyloxy-cyclobutanesulfonic acid [7-(2-fluoro-4-iodo-phenylamino)-6-methyl-5-oxo-1,2,3,5-tetrahydro-imidazo[1,2-a]pyridin-8-yl]-amide

HRID 1259380ノート

反応式

HRID 1259380 の反応式
Cl.O1CCOCC1.C(OC([N:15]1[C:19]2=[C:20]([NH:35][S:36]([CH:39]3[CH2:42][CH:41]([O:43][CH2:44][C:45]4[CH:50]=[CH:49][CH:48]=[CH:47][CH:46]=4)[CH2:40]3)(=[O:38])=[O:37])[C:21]([NH:26][C:27]3[CH:32]=[CH:31][C:30]([I:33])=[CH:29][C:28]=3[F:34])=[C:22]([CH3:25])[C:23](=[O:24])[N:18]2[CH2:17][CH2:16]1)=O)(C)(C)C.CO>C(Cl)(Cl)Cl>[F:34][C:28]1[CH:29]=[C:30]([I:33])[CH:31]=[CH:32][C:27]=1[NH:26][C:21]1[C:20]([NH:35][S:36]([CH:39]2[CH2:42][CH:41]([O:43][CH2:44][C:45]3[CH:46]=[CH:47][CH:48]=[CH:49][CH:50]=3)[CH2:40]2)(=[O:38])=[O:37])=[C:19]2[NH:15][CH2:16][CH2:17][N:18]2[C:23](=[O:24])[C:22]=1[CH3:25]

参加物

5

反応物 3

HCID 887MethanolHCID 204431481,4-Dioxane hydrochlorideHCID 671934168-(3-Benzyloxy-cyclobutanesulfonylamino)-7-(2-fluoro-4-iodo-phenylamino)-6-methyl-5-oxo-2,3-dihydro-5H-imidazo[1,2-a]pyridine-1-carboxylic acid tert-butyl ester

生成物 1

HCID 671942983-Benzyloxy-cyclobutanesulfonic acid [7-(2-fluoro-4-iodo-phenylamino)-6-methyl-5-oxo-1,2,3,5-tetrahydro-imidazo[1,2-a]pyridin-8-yl]-amide収率 55.8%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

Dioxane hydrochloride (3 mL) was added to 8-(3-benzyloxy-cyclobutanesulfonylamino)-7-(2-fluoro-4-iodo-phenylamino)-6-methyl-5-oxo-2,3-dihydro-5H-imidazo[1,2-a]pyridine-1-carboxylic acid tert-butyl ester (250 mg) and the resulting mixture was stirred at room temperature for 12 hours. The reaction was monitored by TLC (5% MeOH in CHCl3). The reaction mixture was concentrated; the concentrate was neutralized with NaHCO3 solution and extracted with ethylacetate. The organic layer was washed with brine, dried over Na2SO4 and concentrated to afford 120 mg of the product (55.8% yield).

後処理

  1. concentrationThe reaction mixture was concentrated
  2. extractionextracted with ethylacetate
  3. washThe organic layer was washed with brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-914b0bb5eef74e848ff3be73f0e0c2f0
出典データセット
uspto-grants-2013_06
特許番号
US08466289B2

反応ノート

読み込み中…