Hydrochloric Acid → HCID 19439680、化合物

HRID 1734021ノート

反応式

HRID 1734021 の反応式
O.NN.C1(=O)[N:8]([CH2:9][C:10]2[CH:11]=[C:12]([C:18](=[O:20])[CH3:19])[CH:13]=[CH:14][C:15]=2[O:16][CH3:17])C(=O)C2=CC=CC=C12.Cl>CO.O1CCCC1>[NH2:8][CH2:9][C:10]1[CH:11]=[C:12]([C:18](=[O:20])[CH3:19])[CH:13]=[CH:14][C:15]=1[O:16][CH3:17]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 24654Hydrazine hydrate (1:1)HCID 3922617HCID 3922617、化合物

生成物 1

HCID 19439680HCID 19439680、化合物収率 48.8%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Hydrazine hydrate (3.06 g) was added to a suspension of 3'-phthalimidomethyl-4'-methoxyacetophenone (15.74 g) in methanol (150 ml) and tetrahydrofuran (150 ml) at room temperature and the mixture was stirred at room temperature for 24 hours. Dilute hydrochloric acid (conc. hydrochloric acid (5 ml) in water (100 ml)) was added slowly to the mixture with cooling and the mixture was stirred at room temperature for 1 hour. The mixture was concentrated. Water (100 ml) was added thereto and the mixture was alkalized to pH 10 with 30% aqueous potassium carbonate solution and extracted with ethyl acetate (300 ml). The extract was dried with magnesium sulfate. The solvent was removed under reduced pressure to afford 3'-aminomethyl-4'-methoxyacetophenone (4.45 g).

後処理

  1. temperaturewith cooling
  2. stirringthe mixture was stirred at room temperature for 1 hour
  3. concentrationThe mixture was concentrated
  4. additionWater (100 ml) was added
  5. extractionextracted with ethyl acetate (300 ml)
  6. dry with materialThe extract was dried with magnesium sulfate
  7. customThe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-09db1c266b91498285a83bd0b0c0e292
出典データセット
uspto-grants-1996_07
特許番号
US05532258

反応ノート

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