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Acetic Acid → HCID 178478115, 화합물

HRID 1655355
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HRID 1655355 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:15]=[CH:16][CH:17]=1)[CH2:5][O:6][C:7]1[CH:14]=[CH:13][C:10]([C:11]#[N:12])=[CH:9][CH:8]=1.[N-:18]=[N+:19]=[N-:20].[Na+].C(O)(=O)C>C(O)CCC>[Cl:1][C:2]1[CH:3]=[C:4]([CH:15]=[CH:16][CH:17]=1)[CH2:5][O:6][C:7]1[CH:14]=[CH:13][C:10]([C:11]2[NH:20][N:19]=[N:18][N:12]=2)=[CH:9][CH:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 176Acetic Acid2회HCID 33557Sodium Azide2회HCID 3402182HCID 3402182, 화합물

생성물 1

HCID 178478115HCID 178478115, 화합물

시약·촉매·용매 1

HCID 2631-Butanol용매2회

실험 절차

To a solution of 5×10-2 mole of 4-(3-chloro benzyloxy) benzonitrile in 20 ml of butanol are added 6.6×10-2 mole of sodium azide and 6.6×10-2 of acetic acid. Then the reaction mixture is heated to reflux for four days. 1 g of sodium azide, 2 g of acetic acid and 10 ml of butanol are added and the medium is again heated for two days at reflux. After concentrating by evaporating the solvent, the residue is taken up in 20 ml of 10% aqueous NaOH. After filtration, the aqueous phase is extracted with ether. By acidification of the alkaline solution using HCl 2N, the expected compound precipitates and is recrystallized in methanol.

후처리

  1. temperatureThen the reaction mixture is heated
  2. temperatureto reflux for four days
  3. temperaturethe medium is again heated for two days
  4. temperatureat reflux
  5. concentrationAfter concentrating
  6. customby evaporating the solvent
  7. filtrationAfter filtration
  8. extractionthe aqueous phase is extracted with ether
  9. customthe expected compound precipitates
  10. customis recrystallized in methanol

출처 및 근거

ORD 기록
ord-ac7acdd1480f43c9a2a9a811baf5f47a
출처 데이터셋
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05250551

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