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 Methoxide → HCID 178462386、化合物

HRID 1936848
ノート
印刷プレビュー

反応式

HRID 1936848 の反応式
C[O-].[Na+].[F:4][C:5]1[C:10]([F:11])=[CH:9][CH:8]=[CH:7][C:6]=1[C@@:12]1([CH2:16][N:17]2[CH:21]=[N:20][CH:19]=[N:18]2)[C@H:14]([CH3:15])[O:13]1.C([S:25][C@@H:26]1[CH2:31][O:30][C@@H:29]([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[O:28][CH2:27]1)(=O)C>CO.C(O)C>[F:4][C:5]1[C:10]([F:11])=[CH:9][CH:8]=[CH:7][C:6]=1[C@:12]([OH:13])([C@H:14]([S:25][C@@H:26]1[CH2:27][O:28][C@@H:29]([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[O:30][CH2:31]1)[CH3:15])[CH2:16][N:17]1[CH:21]=[N:20][CH:19]=[N:18]1
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 10942334Sodium MethoxideHCID 86757717(2R,3S)-2-(2,3-Difluorophenyl)-3-methyl-2-[(1H-1,2,4-triazol-1-yl)methyl]oxiraneHCID 178477153HCID 178477153、化合物

生成物 1

HCID 178462386HCID 178462386、化合物収率 6.6%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒
HCID 887
Methanol
溶媒

実験手順

0.29 ml (1.4 mmol) of a 4.9 M solution of sodium methoxide in methanol were added to a solution of 1.77 g (7.1 mmol) of (2R,3S)-2-(2,3-difluorophenyl)-3-methyl-2-[(1H-1,2,4-triazol-1-yl)methyl]oxirane [prepared as described in Step 7(iv) above] and 2.20 g (9.2 mmol) of trans-5-(acetylthio)-2-phenyl-1,3-dioxane [prepared as described in Japanese Patent Application (Kokai) Hei 8-333350] in 20 ml of ethanol. The resulting mixture was then heated under reflux for 7 hours. After cooling the reaction mixture, it was partitioned between ethyl acetate and an aqueous ammonium chloride solution. The organic layer was washed with saturated aqueous sodium chloride solution and concentrated under reduced pressure to afford 3.65 g of the crude title compound. An aliquot (0.28 g) of the crude residue was purified by chromatography on a silica gel (15 g) column using a 2:5 mixture of ethyl acetate and hexane as eluent to afford 0.21 g of the title compound.

後処理

  1. temperatureThe resulting mixture was then heated
  2. temperatureunder reflux for 7 hours
  3. temperatureAfter cooling the reaction mixture, it
  4. customwas partitioned between ethyl acetate
  5. washThe organic layer was washed with saturated aqueous sodium chloride solution
  6. concentrationconcentrated under reduced pressure
  7. customto afford 3.65 g of the crude title compound
  8. customAn aliquot (0.28 g) of the crude residue was purified by chromatography on a silica gel (15 g) column
  9. additiona 2:5 mixture of ethyl acetate and hexane as eluent

出典と根拠

ORDレコード
ord-0b2f25f4a9c1429390b86ffb98ea1d5b
出典データセット
uspto-grants-2002_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06391903B1

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