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Water → 2-(5-Cyano-3,4-diphenyl-6-oxo-1,6-dihydropyridazin-1-yl) ethyl sulfonic acid hydrate

HRID 463972
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인쇄 미리보기

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HRID 463972 반응식
[C:1]([C:3]1[C:4](=[O:21])[NH:5][N:6]=[C:7]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:8]=1[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)#[N:2].C([O-])([O-])=O.[K+].[K+].O.[Na+].Br[CH2:31][CH2:32][S:33]([O-:36])(=[O:35])=[O:34]>CN(C=O)C>[OH2:21].[C:1]([C:3]1[C:4](=[O:21])[N:5]([CH2:31][CH2:32][S:33]([OH:36])(=[O:35])=[O:34])[N:6]=[C:7]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:8]=1[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)#[N:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 957574-Pyridazinecarbonitrile, 2,3-dihydro-3-oxo-5,6-diphenyl-HCID 236667972-Bromoethanesulfonic acid, sodium salt

생성물 1

HCID 135335102-(5-Cyano-3,4-diphenyl-6-oxo-1,6-dihydropyridazin-1-yl) ethyl sulfonic acid hydrate수율 50.1%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

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온도
110 °C

실험 절차

7.5 grams (0.027 mole) of the product of Example 1 was caused to react with 3.79 grams of K2CO3 in the least amount of water along with 200 mls of DMF. To this mixture was added 5 drops of 18 crown-6-ether. Into this solution was added 5.79 grams (0.027 mole) of 2-bromoethane sulfonic acid sodium salt and the mixture heated to 110° C. for 3 hours. The solution was filtered and the filtrate was distilled at reduced pressure. The residual solid was dissolved in excess water and poured into conc. hydrochloric acid. The solid that precipitated was filtered and washed with water and then air dried. The recovered solid was recrystallized from acetonitrile to give 2.7 grams of a yellow solid which melted at 138°-140° C.

후처리

  1. filtrationThe solution was filtered
  2. distillationthe filtrate was distilled at reduced pressure
  3. dissolutionThe residual solid was dissolved in excess water
  4. additionpoured into conc. hydrochloric acid
  5. customThe solid that precipitated
  6. filtrationwas filtered
  7. washwashed with water
  8. customair dried
  9. customThe recovered solid was recrystallized from acetonitrile

출처 및 근거

ORD 기록
ord-66ac0158d8074536b9b18328140f45bc
출처 데이터셋
uspto-grants-1985_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04545810

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