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 Hydroxide → 5-(3-Hydroxy-1-propynyl)-2,2'-bithiophene

HRID 1599496
ノート
印刷プレビュー

反応式

HRID 1599496 の反応式
[OH:1][C:2]#[C:3][CH3:4].I[C:6]1[S:10][C:9]([C:11]2[S:12][CH:13]=[CH:14][CH:15]=2)=[CH:8][CH:7]=1.[OH-].[Na+].[NH4+].[Cl-]>C1C=CC=CC=1.[Cl-].C([N+](CC)(CC)CC)C1C=CC=CC=1.[Cu]I.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[OH:1][CH2:2][C:3]#[C:4][C:6]1[S:10][C:9]([C:11]2[S:12][CH:13]=[CH:14][CH:15]=2)=[CH:8][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

HCID 14798Sodium HydroxideHCID 25517Ammonium ChlorideHCID 6432594Prop-1-yn-1-olHCID 113237785-Iodo-2,2'-bithiophene

生成物 1

HCID 189204415-(3-Hydroxy-1-propynyl)-2,2'-bithiophene収率 74.3%

試薬・触媒・溶媒 4

HCID 24350
Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
触媒
HCID 66133Benzyl triethylammonium chloride触媒
HCID 178418397HCID 178418397、化合物触媒
HCID 241Benzene溶媒

実験手順

Hydroxy-1-propyne (48 mg) was dissolved in benzene (1 ml). 5-Iodo-2,2'-bithiophene (0.1 g) was added immediately and stirred. A mixture of CuI (0.05 g), benzyltriethylammonium chloride (0.05 g), catalyst Pd(PPh3)4 (0.1 g) and 3 ml of NaOH solution (2.5N) were mixed together at room temperature and stirred for 2 hours. NH4Cl solution (4 ml) was then added. The reaction solution was extracted with ethyl acetate. The extract was washed with 10 ml of HCl (10%) for 3 times, 50 ml of water twice and dried over anhydrous magnesium sulfate. The residual solid was purified by silica gel column chromatography, eluted with ethyl acetate/n-hexane (3/1) to yield 56 mg of the product (74%).

後処理

  1. additionwere mixed together at room temperature
  2. stirringstirred for 2 hours
  3. extractionThe reaction solution was extracted with ethyl acetate
  4. washThe extract was washed with 10 ml of HCl (10%) for 3 times, 50 ml of water twice
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe residual solid was purified by silica gel column chromatography
  7. washeluted with ethyl acetate/n-hexane (3/1)

出典と根拠

ORDレコード
ord-9cdc6e4007b14e97bafd48cf42c7f12d
出典データセット
uspto-grants-1998_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05741811

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