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Methanesulfonic Acid → HCID 57684696、化合物

HRID 1175250
ノート
印刷プレビュー

反応式

HRID 1175250 の反応式
[CH2:1]([O:4][CH2:5][CH2:6][C:7]1[CH:21]=[CH:20][C:10]([CH2:11][C:12]2[CH:17]=[C:16](Br)[CH:15]=[CH:14][C:13]=2[Cl:19])=[CH:9][CH:8]=1)[CH:2]=[CH2:3].[CH2:22]([O:29][C@@H:30]1[C@@H:35]([O:36][CH2:37][C:38]2[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=2)[C@H:34]([O:44][CH2:45][C:46]2[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=2)[C@@H:33]([CH2:52][O:53][CH2:54][C:55]2[CH:60]=[CH:59][CH:58]=[CH:57][CH:56]=2)[O:32][C:31]1=[O:61])[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1.[CH2:62]([Li])CCC.CS(O)(=O)=O.C(=O)(O)[O-].[Na+]>C1COCC1.CCCCCC.CO.O>[CH2:1]([O:4][CH2:5][CH2:6][C:7]1[CH:21]=[CH:20][C:10]([CH2:11][C:12]2[CH:17]=[C:16]([C@@:31]3([O:61][CH3:62])[C@H:30]([O:29][CH2:22][C:23]4[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=4)[C@@H:35]([O:36][CH2:37][C:38]4[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=4)[C@H:34]([O:44][CH2:45][C:46]4[CH:47]=[CH:48][CH:49]=[CH:50][CH:51]=4)[C@@H:33]([CH2:52][O:53][CH2:54][C:55]4[CH:56]=[CH:57][CH:58]=[CH:59][CH:60]=4)[O:32]3)[CH:15]=[CH:14][C:13]=2[Cl:19])=[CH:9][CH:8]=1)[CH:2]=[CH2:3]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

10

反応物 5

HCID 6395Methanesulfonic AcidHCID 516892Sodium BicarbonateHCID 10907626(3R,4S,5R,6R)-3,4,5-Tris(benzyloxy)-6-((benzyloxy)methyl)oxan-2-oneHCID 595577752-(4-(2-(Allyloxy)ethyl)benzyl)-4-bromo-1-chlorobenzeneHCID 178418339Butyllithium

生成物 1

HCID 57684696
HCID 57684696、化合物
収率 28%

試薬・触媒・溶媒 4

HCID 887Methanol溶媒HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒HCID 8058Hexane溶媒

反応条件

温度
-78 °C

実験手順

To a mixture of 2-(4-(2-(allyloxy)ethyl)benzyl)-4-bromo-1-chlorobenzene (intermediate BI) (123 mg, 0.34 mmol) and (3R,4S,5R,6R)-3,4,5-tris(benzyloxy)-6-(benzyloxymethyl)tetrahydro-2H-pyran-2-one (362 mg, 0.67 mmol) in anhydrous THF (1.5 mL) under argon and kept at −78° C. was added dropwise a 1.6 M solution of n-butyl lithium in hexane (0.63 mL) over 15 min. The mixture was stirred at −78° C. for 1.5 h. A solution of methanesulfonic acid (0.1 mL) in methanol (1 mL) was added to the reaction mixture and allowed to warm to room temperature over time. The mixture was stirred at room temperature for 21 h. A saturated solution of sodium bicarbonate was slowly added to the reaction mixture to bring the pH to 8. Water (2 mL) was added and the product was extracted into ethyl acetate (3×2 mL), the combined ethyl acetate solution was washed with brine (1.5 mL), dried (Na2SO4), filtered and evaporated. Preparative thin layer chromatography (TLC) using 12:1 hexane:EtOAc gave intermediate BJ (80 mg, yield 28%). LC-ESI-MS (m/z): 807 (M-OMe).

後処理

  1. customkept at −78° C.
  2. temperatureto warm to room temperature over time
  3. stirringThe mixture was stirred at room temperature for 21 h
  4. extractionthe product was extracted into ethyl acetate (3×2 mL)
  5. washthe combined ethyl acetate solution was washed with brine (1.5 mL)
  6. dry with materialdried (Na2SO4)
  7. filtrationfiltered
  8. customevaporated
  9. customEtOAc gave intermediate BJ (80 mg, yield 28%)

出典と根拠

ORDレコード
ord-8b463d8ac54c4c78b75902cf019bcd24
出典データセット
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07838499B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート