Hydrochloric Acid → HCID 14130307, 화합물

HRID 1708977노트

반응식

HRID 1708977 반응식
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

참가 물질

6

반응물 3

HCID 313Hydrochloric Acid2회HCID 136563003-Chloro-4,5-bis[(prop-2-yn-1-yl)oxy]anilineHCID 23668193Sodium Nitrite

생성물 1

HCID 14130307HCID 14130307, 화합물

시약·촉매·용매 2

HCID 24014Cupric Chloride촉매HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7cb227abb8ba4a65aef7deaa2ec7f528
출처 데이터셋
uspto-grants-1990_08
특허 번호
US04946865

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