Hydrochloric Acid → Hydralazine Hydrochloride

HRID 492104

反応式

HRID 492104 の反応式
[CH:1]1[CH:2]=[CH:3][C:4]2[C:5](=[CH:7][N:8]=[N:9][C:10]=2[NH:11][NH2:12])[CH:6]=1.[ClH:13]>>[CH:1]1[CH:2]=[CH:3][C:4]2[C:5](=[CH:7][N:8]=[N:9][C:10]=2[NH:11][NH2:12])[CH:6]=1.[ClH:13]

参加物

3

反応物 2

HCID 313Hydrochloric AcidHCID 3637Hydralazine

生成物 1

HCID 9351Hydralazine Hydrochloride収率 65%

実験手順

Again according to the disclosure in the '397 application, hydralazine free base 25 g (1 part by weight) was heated in 165 mL (6 to 7 parts by volume) of 15% hydrochloric acid to a temperature of 70-80° C. The solution was filtered hot to remove traces of insoluble materials that were undesired by-products of the preceding step. One hundred sixty five milliliters of ethanol (6 to 7 parts by volume) was added to the filtrate. As the resulting solution cooled to 25° (ambient temperature) and then further cooled to 3-8° C., a pale yellow precipitate of the desired product, hydralazine hydrochloride, solidified. The obtained yield is 65% (the reported yields in the '397 application were 80-90%).

後処理

  1. filtrationThe solution was filtered hot
  2. customto remove traces of insoluble materials that
  3. additionOne hundred sixty five milliliters of ethanol (6 to 7 parts by volume) was added to the filtrate
  4. temperaturefurther cooled to 3-8° C.
  5. customThe obtained yield is 65% (the reported yields in the '397 application

出典と根拠

ORDレコード
ord-1fd7f10b50ba4f04baf3afd03b831b8c
出典データセット
uspto-grants-2009_05
特許番号
US07531653B2

関連ノート

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