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

1,2-Diaminocyclohexane, trans- → 9-(dibenzo[b,d]thiophen-4-yl)-3-fluoro-9H-carbazole

HRID 879914
ノート
印刷プレビュー

反応式

HRID 879914 の反応式
[F:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:6][C:7]3[C:12]([C:13]=2[CH:14]=1)=[CH:11][CH:10]=[CH:9][CH:8]=3.I[C:16]1[C:21]2[S:22][C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=3[C:20]=2[CH:19]=[CH:18][CH:17]=1.P([O-])([O-])([O-])=O.[K+].[K+].[K+].[C@@H]1(N)CCCC[C@H]1N>[Cu]I.O1CCOCC1>[CH:19]1[C:20]2[C:24]3[CH:25]=[CH:26][CH:27]=[CH:28][C:23]=3[S:22][C:21]=2[C:16]([N:6]2[C:5]3[CH:4]=[CH:3][C:2]([F:1])=[CH:14][C:13]=3[C:12]3[C:7]2=[CH:8][CH:9]=[CH:10][CH:11]=3)=[CH:17][CH: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

7

反応物 4

HCID 438061,2-Diaminocyclohexane, trans-HCID 62657Potassium Phosphate, TribasicHCID 4583534-IododibenzothiopheneHCID 158868413-Fluorocarbazole

生成物 1

HCID 867225089-(dibenzo[b,d]thiophen-4-yl)-3-fluoro-9H-carbazole収率 48.1%

試薬・触媒・溶媒 2

HCID 24350
Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
触媒
HCID 312751,4-Dioxane溶媒

実験手順

A mixture of 6.7 g (36.2 mmole) 3-fluoro-9H-carbazole, 11.2 g (36.2 mmole) of 4-iododibenzo[b,d]thiophene, 17.1 g (90 mmole) of copper(I) iodide, 19.1 g (90 mmole) of potassium phosphate, 10.3 g (90 mmole) of trans-1,2-cyclohexanediamine and 1,4-dioxane 700 ml were refluxed under nitrogen for about overnight. Then, the solution was filtered at 110° C. To receive the filtrate, And the 1,4-dioxane was removed under reduced pressure from the filtrate. The filtrate was extracted with 500 ml dichloromethane and 2000 ml water, the organic layer was dried with anhydrous magnesium sulfate, the solvent was removed and the residue was purified by column chromatography on silica (hexane-ethyl acetate) to give product 6.4 g (48%).

後処理

  1. temperaturewere refluxed under nitrogen for about overnight
  2. filtrationThen, the solution was filtered at 110° C
  3. customthe 1,4-dioxane was removed under reduced pressure from the filtrate
  4. extractionThe filtrate was extracted with 500 ml dichloromethane and 2000 ml water
  5. dry with materialthe organic layer was dried with anhydrous magnesium sulfate
  6. customthe solvent was removed
  7. customthe residue was purified by column chromatography on silica (hexane-ethyl acetate)

出典と根拠

ORDレコード
ord-c71573ea9d664314be50bf5f1de4d2dd
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08993130B2

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