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

tert-Butanol → HCID 21099527、化合物

HRID 2377016
ノート
印刷プレビュー

反応式

HRID 2377016 の反応式
Cl[S:2]([N:5]=C=O)(=[O:4])=[O:3].C(O)(C)(C)C.C(N(CC)CC)C.Cl.[F:21][C:22]1[CH:27]=[CH:26][C:25](/[CH:28]=[CH:29]/[C:30]2[CH:35]=[CH:34][C:33]([S:36]([C:39]3[CH:40]=[C:41]([NH2:45])[CH:42]=[CH:43][CH:44]=3)(=[O:38])=[O:37])=[CH:32][CH:31]=2)=[CH:24][CH:23]=1>ClCCl>[F:21][C:22]1[CH:23]=[CH:24][C:25](/[CH:28]=[CH:29]/[C:30]2[CH:31]=[CH:32][C:33]([S:36]([C:39]3[CH:40]=[C:41]([NH:45][S:2]([NH2:5])(=[O:4])=[O:3])[CH:42]=[CH:43][CH:44]=3)(=[O:38])=[O:37])=[CH:34][CH:35]=2)=[CH:26][CH:27]=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 4

HCID 6386tert-ButanolHCID 8471TriethylamineHCID 70918Chlorosulfonyl isocyanateHCID 21099488HCID 21099488、化合物

生成物 1

HCID 21099527HCID 21099527、化合物収率 36%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To dichloromethane (1 mL) at 0° C. was added chlorosulfonyl isocyanate (0.03 mL, 0.26 mmol) and tert-butanol (0.03 mL, 0.26 mmol). The mixture was stirred for 10 minutes then triethylamine (0.054 mL, 0.39 mmol) was added followed by [3-({4-[(E)-2-(4-fluorophenyl)vinyl]phenyl}sulfonyl)phenyl]amine hydrochloride (Example 212, 100 mg, 0.26 mmol). The reaction was allowed to warm to room temperature and stirred for 2 hours. The mixture was partitioned between ethyl acetate and water. The organic layer was washed with brine, dried over MgSO4 and evaporated. The residue was treated with trifluoroacetic acid for 15 minutes then evaporated. The residue was partitioned between ethyl acetate and 1M sodium hydroxide. The organic layer was washed with brine, dried over MgSO4 and evaporated. The residue was purified by flash column chromatography on silica, eluting with 50% ethyl acetate/isohexane to give the title compound (40 mg, 36%). δH (500 MHz, d6 DMSO): 9.94 (1H, s), 7.89 (2H, d, J=8.4 Hz), 7.79 (2H, d, J=8.4 Hz), 7.71-7.65 (3H, m), 7.51-7.48 (2H, m), 7.44-7.38 (2H, m), 7.30-7.20 (5H, m); m/z (ES+) 431 [MH+].

後処理

  1. stirringstirred for 2 hours
  2. customThe mixture was partitioned between ethyl acetate and water
  3. washThe organic layer was washed with brine
  4. dry with materialdried over MgSO4
  5. customevaporated
  6. additionThe residue was treated with trifluoroacetic acid for 15 minutes
  7. customthen evaporated
  8. customThe residue was partitioned between ethyl acetate and 1M sodium hydroxide
  9. washThe organic layer was washed with brine
  10. dry with materialdried over MgSO4
  11. customevaporated
  12. customThe residue was purified by flash column chromatography on silica
  13. washeluting with 50% ethyl acetate/isohexane

出典と根拠

ORDレコード
ord-5e4eea1ccfa44cc5af8e47ec614c8260
出典データセット
uspto-grants-2008_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07468393B2

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