Hydrochloric Acid → 9-Ethynyl-9-fluorenol

HRID 2294275ノート

反応式

HRID 2294275 の反応式
[CH:1]1[C:13]2[C:12](=[O:14])[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.[CH2:15]1COC[CH2:16]1.[C-]#[C-].[Na+].[Na+].Cl>C1(C)C(C)=CC=CC=1>[C:15]([C:12]1([OH:14])[C:13]2[CH:1]=[CH:2][CH:3]=[CH:4][C:5]=2[C:6]2[C:11]1=[CH:10][CH:9]=[CH:8][CH:7]=2)#[CH:16]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 10241FluorenoneHCID 178463197HCID 178463197、化合物

生成物 1

HCID 5187719-Ethynyl-9-fluorenol

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

9 g (0.05 mol) of 9-fluorenone and 100 ml of anhydrous THF are charged into a dry flask of 250 ml. To the resulting solution a suspension of sodium acetylide [17.8 g (0.0525 mol) in mineral oil/xylene, 18% by weight based on the suspension; solid purity 95%] is added under nitrogen, by means of a syringe. The resulting suspension is kept overnight under nitrogen and with stirring before being poured into 75 ml of 10% HCl. The phases are separated and the aqueous phase is extracted twice with 100 ml of ethyl ether. The organic extracts are combined and thoroughly dried over sodium sulfate. By eliminating the solvent, 10.1 g of product is obtained, which is used without any further purification.

後処理

  1. additionsolid purity 95%] is added under nitrogen, by means of a syringe
  2. customThe phases are separated
  3. extractionthe aqueous phase is extracted twice with 100 ml of ethyl ether
  4. dry with materialthoroughly dried over sodium sulfate

出典と根拠

ORDレコード
ord-c5d223da2d444ae0a8da41efee7ae32b
出典データセット
uspto-grants-1997_11
特許番号
US05688846

反応ノート

読み込み中…