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 1259380노트

반응식

HRID 1259380 반응식
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]

참가 물질

5

반응물 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

생성물 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]-amide수율 55.8%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-914b0bb5eef74e848ff3be73f0e0c2f0
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08466289B2

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