Hydrazine hydrate (1:1) → Hydralazine

HRID 492106

반응식

HRID 492106 반응식
O.[NH2:2][NH2:3].Cl[C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[CH:8]=[N:7][N:6]=1>CO>[CH:11]1[CH:12]=[CH:13][C:14]2[C:9](=[CH:8][N:7]=[N:6][C:5]=2[NH:2][NH2:3])[CH:10]=1

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 1607931-Chlorophthalazine

생성물 1

HCID 3637Hydralazine수율 99%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
2.5 °C

실험 절차

A 2 L, 3-necked, round-bottomed flask fitted with a temperature probe and condenser, and was charged 375 mL of hydrazine hydrate; the solution was then cooled to 0 to 5° C. About 75 g of 1-chlorophthalazine salt was added in portions at a rate to maintain the solution temperature at 0 to 5° C. After addition, the solution was stirred at 20 to 25° C. for about 24 hrs. The reaction mixture was then cooled to 0 to 5° C. and 150 mL of methanol was added, the solution stirred for 3 hrs, and the resulting solid material was filtered, washed with 150 mL of cold methanol, and dried under vacuum at 35° C. Yield 99%.

후처리

  1. customA 2 L, 3-necked, round-bottomed flask fitted with a temperature probe and condenser
  2. temperatureto maintain the solution temperature at 0 to 5° C
  3. additionAfter addition
  4. temperatureThe reaction mixture was then cooled to 0 to 5° C.
  5. stirringthe solution stirred for 3 hrs
  6. filtrationthe resulting solid material was filtered
  7. washwashed with 150 mL of cold methanol
  8. customdried under vacuum at 35° C

출처 및 근거

ORD 기록
ord-35f0bfb01b28422585845fb955d5cc72
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07531653B2

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