Hydrochloric Acid → HCID 14130307、化合物

HRID 1708977ノート

反応式

HRID 1708977 の反応式
N([O-])=O.[Na+].[Cl:5][C:6]1[CH:7]=[C:8]([CH:10]=[C:11]([O:17][CH2:18][C:19]#[CH:20])[C:12]=1[O:13][CH2:14][C:15]#[CH:16])N.[ClH:21]>C(O)(=O)C.[Cu](Cl)Cl>[Cl:21][C:8]1[CH:10]=[C:11]([O:17][CH2:18][C:19]#[CH:20])[C:12]([O:13][CH2:14][C:15]#[CH:16])=[C:6]([Cl:5])[CH:7]=1

参加物

6

反応物 3

HCID 313Hydrochloric Acid2 回HCID 136563003-Chloro-4,5-bis[(prop-2-yn-1-yl)oxy]anilineHCID 23668193Sodium Nitrite

生成物 1

HCID 14130307HCID 14130307、化合物

試薬・触媒・溶媒 2

HCID 24014Cupric Chloride触媒HCID 176Acetic Acid溶媒

実験手順

Sodium nitrite (1.33 g) was added to a solution of 3-chloro-4,5-dipropargyloxyaniline (4.47 g) in acetic acid (30 ml) and 35% hydrochloric acid (4 ml) at 0° C., followed by stirring at the same temperature for 1 hour. The resultant solution was poured into 35% hydrochloric acid (20 ml) containing copper chloride (2.35 g) at room temperature, and stirring was continued at 60° C. for 30 minutes. The reaction mixture was poured into ice-water and extracted with ethyl acetate. The extract was washed with aqueous sodium carbonate solution, dried over magnesium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel chromatography using toluene as an eluent to give 1,3-dichloro-4,5-dipropargyloxybenzene (3.60 g) as white crystals. m.p. 61°-63° C.

後処理

  1. stirringstirring
  2. waitwas continued at 60° C. for 30 minutes
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with aqueous sodium carbonate solution
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-7cb227abb8ba4a65aef7deaa2ec7f528
出典データセット
uspto-grants-1990_08
特許番号
US04946865

反応ノート

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