Hydrochloric Acid → Lesopitron dihydrochloride

HRID 362778ノート

反応式

HRID 362778 の反応式
[CH:1]1[CH:2]=[N:3][C:4]([N:7]2[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][CH2:15][CH2:16][N:17]3[N:21]=[CH:20][C:19]([Cl:22])=[CH:18]3)[CH2:9][CH2:8]2)=[N:5][CH:6]=1.[ClH:23]>C(O)(C)C>[CH2:9]1[N:10]([CH2:13][CH2:14][CH2:15][CH2:16][N:17]2[N:21]=[CH:20][C:19]([Cl:22])=[CH:18]2)[CH2:11][CH2:12][N:7]([C:4]2[N:3]=[CH:2][CH:1]=[CH:6][N:5]=2)[CH2:8]1.[ClH:23].[ClH:22]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 60813Lesopitron

生成物 1

HCID 60812Lesopitron dihydrochloride収率 195.5%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

A 250 L enamelled reactor was loaded with an isopropanolic solution (57 Kg) of Lesopitron (25.2 mol), and was cooled to 5°-10° C. Subsequently, 8.5 Kg of a solution of hydrochloric acid (58.3 mol) in isopropanol were added, keeping the temperature between 5° and 15° C. during the addition. After stirring the suspension for 30 minutes, the product was centrifuged and washed with isopropanol. The Lesopitron dihydrochloride was washed and then dried in an air oven at 40° C. for 15 hours, obtaining 9.7 Kg (98% yield) of the compound mentioned in the title.

後処理

  1. temperaturewas cooled to 5°-10° C
  2. customthe temperature between 5° and 15° C.
  3. additionduring the addition
  4. washwashed with isopropanol
  5. washThe Lesopitron dihydrochloride was washed
  6. customdried in an air oven at 40° C. for 15 hours

出典と根拠

ORDレコード
ord-57d25957bbf443e6b00767cf1aa41038
出典データセット
uspto-grants-1999_02
特許番号
US05872125

反応ノート

読み込み中…