Hydrazine hydrate (1:1) → Hydralazine

HRID 1158224

反応式

HRID 1158224 の反応式
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>C(O)C>[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

参加物

4

反応物 2

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

生成物 1

HCID 3637Hydralazine収率 80%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
50 °C

実験手順

Again according to the disclosure in the '397 application, to a 2-L, 3-necked, round-bottomed flask fitted with a temperature probe and condenser were charged 700 mL of ethanol and 7.6 mole equivalents (630 mL) of hydrazine hydrate, and the solution was cooled to 50° C. (the '397 application discloses a temperature <10° C.). One (1) mole equivalent (280 g) of 1-chlorophthalazine (solid) was added in portions at a rate to maintain the solution temperature at <20° C. The solution was stirred and heated to 60-70° C. After one hour at that elevated temperature, the hot solution was filtered to remove any insoluble by-products (insoluble matter recovered was 12 g), and the filtrate was cooled to 0 to 5° C. A light yellow solid formed in the cold solution, which was isolated by filtration, washed with cold ethanol, and then dried to constant mass and characterized. The yield was 80% (the yield reported in the '397 application was 77-80%).

後処理

  1. temperatureto maintain the solution temperature at <20° C
  2. temperatureheated to 60-70° C
  3. filtrationthe hot solution was filtered
  4. customto remove
  5. customany insoluble by-products (insoluble matter recovered was 12 g)
  6. temperaturethe filtrate was cooled to 0 to 5° C
  7. customA light yellow solid formed in the cold solution
  8. customwhich was isolated by filtration
  9. washwashed with cold ethanol
  10. customdried to constant mass

出典と根拠

ORDレコード
ord-bb6d8be684774c60a3910db54716eeaf
出典データセット
uspto-grants-2010_10
特許番号
US07807830B2

関連ノート

読み込み中…