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

Chloroacetyl chloride → HCID 69701133、化合物

HRID 1596091
ノート
印刷プレビュー

反応式

HRID 1596091 の反応式
C1(C)C=CC(S(Cl)(=O)=O)=CC=1.[Cl:12][C:13]1[CH:14]=[C:15]([CH:20](O)[C@H:21]([OH:44])[CH2:22][CH2:23][O:24][C:25]([C:38]2[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=2)([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[CH:16]=[CH:17][C:18]=1[Cl:19].O.O.O.Cl([O-])(=O)(=O)=O.[Li+].[CH:55]1([CH2:61][NH2:62])[CH2:60][CH2:59][CH2:58][CH2:57][CH2:56]1.C(N(CC)CC)C.[Cl:70][CH2:71][C:72](Cl)=[O:73]>N1C=CC=CC=1.C(Cl)Cl.C(OCC)(=O)C.O>[C:38]1([C:25]([C:32]2[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=2)([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[O:24][CH2:23][CH2:22][C@@H:21]([OH:44])[CH:20]([C:15]2[CH:16]=[CH:17][C:18]([Cl:19])=[C:13]([Cl:12])[CH:14]=2)[N:62]([C:72](=[O:73])[CH2:71][Cl:70])[CH2:61][CH:55]2[CH2:60][CH2:59][CH2:58][CH2:57][CH2:56]2)[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

11

反応物 6

HCID 6577Chloroacetyl chlorideHCID 73974-Toluenesulfonyl chlorideHCID 8471TriethylamineHCID 76688CyclohexanemethylamineHCID 23708903Lithium perchlorate trihydrateHCID 53669173HCID 53669173、化合物

生成物 1

HCID 69701133
HCID 69701133、化合物
収率 63%

試薬・触媒・溶媒 4

HCID 962Water溶媒HCID 1049Pyridine溶媒HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

p-Toluenesulfonyl chloride (2.03g, 10.7 mmol) was added to a solution of (2R)-(3,4-dichlorophenyl)-4-(triphenylmethoxy)butan-1,2-diol (3.51 g, 7.11 mmol), which was prepared in Example 12(a), in pyridine (17 ml). The mixture was stirred at room temperature overnight. To the reaction mixture, water was added and it was extracted with ethyl acetate. The organic layer was dried over anydrous magnesium sulfate and then the solvent was distilled off under reduced pressure. The residue was dissolved in acetonitrile (50 ml) and lithium perchlorate trihydrate (3.42 g. 21.3 mmol) and cyclohexylmethylamine (2.78 ml, 21.3 mmol) were added to the solution. The mixture was stirred at 100° C. overnight. Ethyl acetate was added to the reaction mixture and it was washed with a saturated aqueous solution of sodium chloride. The organic layer was dried over anhydrous magnesium sulfate and then the solvent was distilled off under reduced pressure. A half of the residue by weight was dissolved in methylene chloride (30 ml). To this solution, triethylamine (2.48 ml, 17.8 mmol) and chloroacetyl chloride (1.42 ml, 17.8 mmol) were added with ice-cooling. The mixture was stirred at 0° C. for 1 hour. To the reaction mixture, methylene chloride was added, the organic layer was washed with water and then with a saturated aquoeus solution of sodium chloride and was dried over anhydrous magnesium sulfate. After distillation under reduced pressure, the resulting residue was purified by flash chromatography on a silica gel column using n-hexane/ethyl acetate=20/1−10/1 as an eluant to afford the title compound (1.49 g, 63%).

後処理

  1. extractionit was extracted with ethyl acetate
  2. dry with materialThe organic layer was dried over anydrous magnesium sulfate
  3. distillationthe solvent was distilled off under reduced pressure
  4. dissolutionThe residue was dissolved in acetonitrile (50 ml)
  5. stirringThe mixture was stirred at 100° C. overnight
  6. washwas washed with a saturated aqueous solution of sodium chloride
  7. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  8. distillationthe solvent was distilled off under reduced pressure
  9. dissolutionA half of the residue by weight was dissolved in methylene chloride (30 ml)
  10. temperaturecooling
  11. stirringThe mixture was stirred at 0° C. for 1 hour
  12. washthe organic layer was washed with water
  13. dry with materialwith a saturated aquoeus solution of sodium chloride and was dried over anhydrous magnesium sulfate
  14. distillationAfter distillation under reduced pressure
  15. customthe resulting residue was purified by flash chromatography on a silica gel column

出典と根拠

ORDレコード
ord-923e8a331ff8427a91628567e3f39522
出典データセット
uspto-grants-2001_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06288059B1

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