ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Sodium Iodide → HCID 11445358、化合物

HRID 915295
ノート
印刷プレビュー

反応式

HRID 915295 の反応式
Cl[CH:2]([O:4][C:5](=[O:32])[N:6]([C:29](=[O:31])[CH3:30])[CH2:7][C@@H:8]1[O:12][C:11](=[O:13])[N:10]([C:14]2[CH:19]=[CH:18][C:17]([CH:20]3[CH2:25][CH2:24][S:23](=[O:27])(=[O:26])[CH2:22][CH2:21]3)=[C:16]([F:28])[CH:15]=2)[CH2:9]1)[CH3:3].[Cs].[C:34]([NH:41][C@H:42]([C:47]([OH:49])=[O:48])[C@H:43]([CH2:45][CH3:46])[CH3:44])([O:36][C:37]([CH3:40])([CH3:39])[CH3:38])=[O:35].[I-].[Na+]>O.C(#N)C>[C:29]([N:6]([CH2:7][C@@H:8]1[O:12][C:11](=[O:13])[N:10]([C:14]2[CH:19]=[CH:18][C:17]([CH:20]3[CH2:25][CH2:24][S:23](=[O:27])(=[O:26])[CH2:22][CH2:21]3)=[C:16]([F:28])[CH:15]=2)[CH2:9]1)[C:5]([O:4][CH:2]([O:49][C:47](=[O:48])[C@@H:42]([NH:41][C:34]([O:36][C:37]([CH3:38])([CH3:40])[CH3:39])=[O:35])[C@@H:43]([CH3:44])[CH2:45][CH3:46])[CH3:3])=[O:32])(=[O:31])[CH3:30]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 5238Sodium IodideHCID 2724762tert-Butoxycarbonyl-L-isoleucineHCID 5354618CesiumHCID 58958558HCID 58958558、化合物

生成物 1

HCID 11445358HCID 11445358、化合物収率 79%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6342Acetonitrile溶媒

実験手順

Acetyl-{3-[4-(1,1-dioxo-hexahydro-1λ6-thiopyran-4-yl)-3-fluoro-phenyl]-2-oxo-oxazolidin-5(R)-ylmethyl}-carbamic acid 1-chloro-ethyl ester (11) (1.00 g, 2.04 mmol), the cesium salt of N-BOC-L-isoleucine (15f) (1.48 g, 4.07 mmol), sodium iodide (0.31 g, 2.07 mmol) and acetonitrile (50 mL) are heated to reflux overnight. After cooling to RT, water is added and the reaction mixture is extracted with EtOAc and then with dichloromethane. The organic phases are washed separately with brine and then the organic layers are combined, dried over MgSO4, filtered, and conc in vacuo. The isolated residue is subjected to silica gel flash chromatography, eluting with MeOH/CH2Cl2 gradient (0-4% MeOH over 1 hour and 30 minutes) to afford the title compound. Isolated yield: 79%. 1H NMR (400 MHz, CDCl3): δ 7.48-7.42 (m, 1H), 7.22-7.17 (m, 1H), 7.14-7.10 (m, 1H), 6.91-6.85 (m, 1H), 5.08 (d, 0.5H), 4.94 (d, 0.5H), 4.81-4.74 (m, 1H), 4.24-3.98 (m, 4H), 3.71-3.64 (m, 1H), 3.13-3.04 (m, 5H), 2.51 (d, 3H), 2.42-2.31 (m, 2H), 2.17-2.13 (m, 2H), 1.84-1.81 (br m, 1H), 1.57 (dd, 3H), 1.52 (s, 1H), 1.38 (d, 9H), 1.21-1.09 (m, 1H), 0.93-0.85 (m, 6H); MS-APCI (m/z+): 341, 385, 586, 686.

後処理

  1. temperatureto reflux overnight
  2. extractionthe reaction mixture is extracted with EtOAc
  3. washThe organic phases are washed separately with brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. washeluting with MeOH/CH2Cl2 gradient (0-4% MeOH over 1 hour and 30 minutes)

出典と根拠

ORDレコード
ord-57343c5487504a5297fbfb6e53e2dd40
出典データセット
uspto-grants-2007_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07265140B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート