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

Dimethyl Sulfate → 2-Methoxy-5-methyl-1-(trifluoromethyl)naphthalene

HRID 615519
ノート
印刷プレビュー

反応式

HRID 615519 の反応式
[CH3:1]OS(OC)(=O)=O.[CH3:8][C:9]1[CH:18]=[CH:17][CH:16]=[C:15]2[C:10]=1[CH:11]=[CH:12][C:13]([OH:23])=[C:14]2[C:19]([F:22])([F:21])[F:20].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH3:1][O:23][C:13]1[CH:12]=[CH:11][C:10]2[C:15](=[CH:16][CH:17]=[CH:18][C:9]=2[CH3:8])[C:14]=1[C:19]([F:20])([F:21])[F:22]
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

5

反応物 3

HCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 155687605-Methyl-1-(trifluoromethyl)naphthalen-2-ol

生成物 1

HCID 155687612-Methoxy-5-methyl-1-(trifluoromethyl)naphthalene収率 90%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
25 °C

実験手順

Dimethylsulfate (1.13 g, 8.75 mmol, 0.85 mL) was added to a stirred suspension of 5-methyl-1-(trifluoromethyl)-2-naphthalenol (1.8 g, 7.96 mmol) and potassium carbonate (2.2 g, 15.9 mmol) in dimethylformamide (20 mL). After stirring the reaction mixture for 2 hr at 25° C. the solid in the reaction mixture was removed by filtration. The filtrate was extracted with hexane (400 mL). The extract was washed with brine, dried (MgSO4) and concentrated to dryness giving 1.7 g (90% yield) of the title compound. This product was used for the reaction described in the next example. A sample of the product, recrystallized from hexane, had mp 70°-71° C.; nmr (CDCl3) 67 2.65 (s, 3H), 3.95 (s, 3H), 7.2 (m, 2H), 7.35 (q, J=8 Hz, 1H), 8.0 (m, 1H), 8.1 (d, J=9 Hz, 1H); ir (CHCl3) 1390, 1340, 1280, 1255, 1245, 1110, 1095, 1085, 1045 cm-1 ; uvλmax (MeOH) 336 nm (ε 2,910), 323 (2,645), 297 (4,440), 286 (4,880), 236 (30,050), 224 (46,730).

後処理

  1. customwas removed by filtration
  2. extractionThe filtrate was extracted with hexane (400 mL)
  3. washThe extract was washed with brine
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-fdf936f284b24136ab501a579d9ec4c4
出典データセット
uspto-grants-1985_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04499310

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