Hexane → HCID 20539488, 화합물

HRID 224995

반응식

HRID 224995 반응식
Cl[C:2]1[N:3]=[N:4][C:5](Cl)=[CH:6][CH:7]=1.[C:9]1([P:15]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[O:16]C)[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.[CH3:24][CH2:25][CH2:26][CH2:27][CH2:28][CH3:29]>ClC1C=CC=CC=1Cl>[C:9]1([P:15]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)([C:2]2[N:3]=[N:4][C:5]([P:15]([C:9]3[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=3)([C:26]3[CH:25]=[CH:24][CH:29]=[CH:28][CH:27]=3)=[O:16])=[CH:6][CH:7]=2)=[O:16])[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1

참가 물질

5

반응물 3

HCID 8058HexaneHCID 673313,6-DichloropyridazineHCID 77636Methoxydiphenylphosphine

생성물 1

HCID 20539488HCID 20539488, 화합물

시약·촉매·용매 1

HCID 72391,2-Dichlorobenzene용매

실험 절차

To a stirred, refluxing solutionof 3.00 g of 3,6-dichloropyridazine in 50 ml of o-dichlorobenzene under nitrogen was added dropwise 10.00 g of methyl diphenylphosphinite. After the addition was completed, the mixture was refluxed for 7 hours and then cooled. The cooled mixture was mixed with excess hexane; the oil which formed slowly crystallized. The resultant solid was separated by filtration, washed with hexane, and recrystallized twice from ethanol with decolorizing charcoal treatment to give 0.93 g of 3,6-bis-(diphenylphosphinyl)pyridazine (shown by formula in Claim 14) as slightly off-white crystals, mp 248°-251.5° C. Anal. Calcd for C28H22N2O2P2 : C, 70.00; H, 4.62; N, 5.83; P, 12.89. Found: C, 69.72; H, 4.92; N, 5.78; P, 12.82.

후처리

  1. additionAfter the addition
  2. temperaturethe mixture was refluxed for 7 hours
  3. temperaturecooled
  4. customthe oil which formed slowly
  5. customcrystallized
  6. customThe resultant solid was separated by filtration
  7. washwashed with hexane
  8. customrecrystallized twice from ethanol with decolorizing charcoal treatment

출처 및 근거

ORD 기록
ord-280ff5bb507745b8a324e341cf0b8fe7
출처 데이터셋
uspto-grants-1980_11
특허 번호
US04234729

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