Lithium Hydroxide → HCID 86728307、化合物

HRID 1776929ノート

反応式

HRID 1776929 の反応式
[F:1][C:2]1[C:3]2[C:4]([CH:45]([OH:51])[C:46]([O:48]CC)=[O:47])=[C:5]3[C:14]4[N:15]=[C:16]([C:19]5[C:20]([N:39]([CH3:44])[S:40]([CH3:43])(=[O:42])=[O:41])=[CH:21][C:22]6[O:26][C:25]([C:27]7[CH:32]=[CH:31][C:30]([F:33])=[CH:29][CH:28]=7)=[C:24]([C:34](=[O:37])[NH:35][CH3:36])[C:23]=6[CH:38]=5)[CH:17]=[CH:18][C:13]=4[O:12][CH2:11][N:6]3[C:7]=2[CH:8]=[CH:9][CH:10]=1.[OH-].[Li+]>C1COCC1.O.CO>[F:1][C:2]1[C:3]2[C:4]([CH:45]([OH:51])[C:46]([OH:48])=[O:47])=[C:5]3[C:14]4[N:15]=[C:16]([C:19]5[C:20]([N:39]([CH3:44])[S:40]([CH3:43])(=[O:42])=[O:41])=[CH:21][C:22]6[O:26][C:25]([C:27]7[CH:28]=[CH:29][C:30]([F:33])=[CH:31][CH:32]=7)=[C:24]([C:34](=[O:37])[NH:35][CH3:36])[C:23]=6[CH:38]=5)[CH:17]=[CH:18][C:13]=4[O:12][CH2:11][N:6]3[C:7]=2[CH:8]=[CH:9][CH:10]=1

参加物

6

反応物 2

HCID 3939Lithium HydroxideHCID 86728306HCID 86728306、化合物

生成物 1

HCID 86728307HCID 86728307、化合物

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of ethyl 2-(11-fluoro-2-(2-(4-fluorophenyl)-3-(methylcarbamoyl)-6-(N-methylmethylsulfonamido)benzofuran-5-yl)-6H-pyrido[2′,3′:5,6][1,3]oxazino[3,4-a]indol-12-yl)-2-hydroxyacetate (233 mg, 0.325 mmol) and lithium hydroxide (54.5 mg, 2.276 mmol) in THF (1 ml), water (0.5 ml) and MeOH (0.5 ml) was stirred at room temperature over night, then concentrated under vacuum. The resulting residue was purified using EP column (30 mm×250 mm), 60% IPA/CO2. This resulted in 128 mg (57.2%) of 2-(11-fluoro-2-(2-(4-fluorophenyl) -3-(methylcarbamoyl)-6-(N-methylmethylsulfonamido)benzofuran-5-yl)-6H-pyrido[2′,3′:5,6][1,3]oxazino[3,4-a]indol-12-yl)-2-hydroxyacetic acid (Compound 207) as a white solid. LC-MS (ES, m/z) C34H26F2N4O8S: 688. Found: 689 [M+H]+.

後処理

  1. concentrationconcentrated under vacuum
  2. customThe resulting residue was purified

出典と根拠

ORDレコード
ord-1c6374b4ec3342d7ac1012d63de8e280
出典データセット
uspto-grants-2016_02
特許番号
US09265773B2

反応ノート

読み込み中…