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 hydride → N-(2,4-dimethylphenyl)-N-isobutyl-4-(((tetrahydro-2H-pyran-4-yl)methoxy)methyl)benzenesulfonamide

HRID 1487053
ノート
印刷プレビュー

反応式

HRID 1487053 の反応式
Br[CH2:2][C:3]1[CH:8]=[CH:7][C:6]([S:9]([N:12]([C:17]2[CH:22]=[CH:21][C:20]([CH3:23])=[CH:19][C:18]=2[CH3:24])[CH2:13][CH:14]([CH3:16])[CH3:15])(=[O:11])=[O:10])=[CH:5][CH:4]=1.[O:25]1[CH2:30][CH2:29][CH:28]([CH2:31][OH:32])[CH2:27][CH2:26]1.[H-].[Na+]>CC1CCCO1.CS(C)=O.ClCCl.O>[CH3:24][C:18]1[CH:19]=[C:20]([CH3:23])[CH:21]=[CH:22][C:17]=1[N:12]([CH2:13][CH:14]([CH3:16])[CH3:15])[S:9]([C:6]1[CH:5]=[CH:4][C:3]([CH2:2][O:32][CH2:31][CH:28]2[CH2:29][CH2:30][O:25][CH2:26][CH2:27]2)=[CH:8][CH:7]=1)(=[O:10])=[O:11]
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

8

反応物 3

HCID 24758Sodium hydrideHCID 2773573(Oxan-4-yl)methanolHCID 867315854-(bromomethyl)-N-(2,4-dimethylphenyl)-N-isobutylbenzenesulfonamide

生成物 1

HCID 72190215N-(2,4-dimethylphenyl)-N-isobutyl-4-(((tetrahydro-2H-pyran-4-yl)methoxy)methyl)benzenesulfonamide

試薬・触媒・溶媒 4

HCID 679Dimethyl Sulfoxide溶媒
HCID 962
Water
溶媒
HCID 6344Dichloromethane溶媒
HCID 73012-Methyltetrahydrofuran溶媒

反応条件

温度
20 °C

実験手順

To a solution of crude 4-(bromomethyl)-N-(2,4-dimethylphenyl)-N-isobutylbenzenesulfonamide (100 mg, 0.122 mmol) and (tetrahydro-2H-pyran-4-yl)methanol (14.15 mg, 0.122 mmol) in 2-methyltetrahydrofuran (2-MeTHF) (1 mL) and dimethyl sulfoxide (DMSO) (0.5 mL) was added sodium hydride (approximately 4.87 mg, 0.122 mmol, 60% dispersed in oil) in one charge. The reaction mixture was stirred at 20° C. for 16 hours. The reaction was then quenched with methanol (0.5 mL) and water (0.5 mL) and concentrated in vacuo to give a residue in DMSO. This was diluted with dichloromethane (10 mL) and water (10 mL) and stirred vigorously for 10 minutes. The layers were separated by hydrophobic frit and the organic fraction evaporated to give the crude product. The sample was then purified by mass directed autoprep (formic acid modifier). The appropriate fractions were concentrated under a stream of nitrogen to give the required product, 4.2 mg. LCMS [LCMS1] Rt 1.44 min, m/z (ES+) 446 (M+H).

後処理

  1. additioncharge
  2. customThe reaction was then quenched with methanol (0.5 mL) and water (0.5 mL)
  3. concentrationconcentrated in vacuo
  4. customto give a residue in DMSO
  5. stirringstirred vigorously for 10 minutes
  6. customThe layers were separated by hydrophobic frit
  7. customthe organic fraction evaporated
  8. customto give the crude product
  9. customThe sample was then purified by mass
  10. concentrationThe appropriate fractions were concentrated under a stream of nitrogen

出典と根拠

ORDレコード
ord-9506c3f27c74452791882c3d7d25c153
出典データセット
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09428452B2

反応ノート

読み込み中…

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