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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
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Methyl iodide → HCID 131710137、化合物

HRID 372621
ノート
印刷プレビュー

反応式

HRID 372621 の反応式
[CH3:1][CH2:2][C@@H:3]([C:22]([C@H:24]([C@@H:26]([OH:42])[C@@H:27]([CH2:29][CH2:30][C:31]1[CH:36]=[CH:35][C:34]([CH3:37])=[C:33]([OH:38])[C:32]=1[C:39]([OH:41])=[O:40])[CH3:28])[CH3:25])=[O:23])[C@H:4]1[O:8][C@@:7]([C@@H:11]2[O:16][C@@H:15]([CH3:17])[C@@:14]([OH:20])([CH2:18][CH3:19])[CH2:13][CH2:12]2)([CH2:9][CH3:10])[CH2:6][C@@H:5]1[CH3:21].[CH2:43](Cl)Cl.CI>[Ag]=O.CO>[CH3:37][C:34]1[CH:35]=[CH:36][C:31]([CH2:30][CH2:29][CH:27]([CH3:28])[CH:26]([OH:42])[CH:24]([CH3:25])[C:22](=[O:23])[CH:3]([CH2:2][CH3:1])[CH:4]2[CH:5]([CH3:21])[CH2:6][C:7]([CH2:9][CH3:10])([CH:11]3[CH2:12][CH2:13][C:14]([CH2:18][CH3:19])([OH:20])[CH:15]([CH3:17])[O:16]3)[O:8]2)=[C:32]([C:39]([O:41][CH3:43])=[O:40])[C:33]=1[OH:38]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6328Methyl iodideHCID 6344DichloromethaneHCID 5360807Lasalocid

生成物 1

HCID 131710137HCID 131710137、化合物

試薬・触媒・溶媒 2

HCID 92152Silver(II) oxide触媒HCID 887Methanol溶媒

実験手順

To a solution of 6.2 g. of crystalline antibiotic X-537A in 125 ml. of methylene chloride was added 4.6 g. of silver oxide and 14 g. of methyl iodide. After stirring for 18 hours, the reaction mixture was filtered and the filtrate concentrated to 7.07 g. of a light yellow oil, which was decolorized with Darco, giving 6.09 g. of a colorless foam. A portion (4 g.) of the foam was chromatographed on a florisil column (150 g.) eluting with a gradient between methylene chloride (1 l.) to ether (1 l.) and then ether (500 ml.) to acetone (500 ml.). Rechromatography of the slightly yellow oil, recovered from the florisil column, on a 75 g. silica gel column and eluting with a gradient between methylene chloride (1 l.) and 15 percent ether/-methylene chloride gave 200 mg. of a clear viscous oil, Bp. 170°d/005 mm. [α] D25 -7.19° , (1.1 percent CH3OH).

後処理

  1. filtrationthe reaction mixture was filtered
  2. concentrationthe filtrate concentrated to 7.07 g
  3. customgiving 6.09 g
  4. customA portion (4 g.) of the foam was chromatographed on a florisil column (150 g.)
  5. washeluting with a gradient between methylene chloride (1 l.) to ether (1 l.)
  6. customRechromatography of the slightly yellow oil, recovered from the florisil column, on a 75 g
  7. washsilica gel column and eluting with a gradient between methylene chloride (1 l.) and 15 percent ether/-methylene chloride
  8. customgave 200 mg

出典と根拠

ORDレコード
ord-5589b77f734a4aae9bb73d9cd7ac7bf9
出典データセット
uspto-grants-1978_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
USRE029651

反応ノート

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