Ammonia → HCID 20359294、化合物

HRID 2083173ノート

反応式

HRID 2083173 の反応式
[OH-].[NH4+].O.[CH3:4][N:5]([CH3:25])[CH2:6][CH2:7][C:8]1([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH2:18][C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[C:10](=[O:11])[O:9]1.N>[Zn].C(O)C>[CH3:25][N:5]([CH3:4])[CH2:6][CH2:7][CH:8]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[CH2:18][C:17]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[C:10]([OH:11])=[O:9]

参加物

7

反応物 4

HCID 222AmmoniaHCID 962WaterHCID 14923Ammonium HydroxideHCID 101085553-(2-Dimethylaminoethyl)-3,4-dihydro-3-phenylisocoumarin

生成物 1

HCID 20359294HCID 20359294、化合物

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 702Ethanol溶媒

実験手順

To a well stirred suspension of 45 g. of zinc dust, 90 ml. of concentrated ammonium hydroxide, 45 ml. of water and 2 ml. of cupric sulfate maintained at 80° C. there is added 14.75 g. (0.05 mole) of 3-(2-dimethylaminoethyl)-3,4-dihydro-3-phenylisocoumarin in 50 ml. ethanol for about 30 minutes. The resulting mixture is heated at 85° C. for 30 hours while a slow stream of ammonia is passed through. The mixture is filtered while under heat and the solids washed throughly with 100 ml. of hot ammonium hydroxide. The combined filtrates are cooled and carefully acidified with concentrated hydrochloric acid to give 2-(β-[-2-dimethylaminoethyl]phenethyl)benzoic acid, m.p. 152° to 154° C.

後処理

  1. additionsuspension of 45 g
  2. additionthere is added 14.75 g
  3. filtrationThe mixture is filtered while
  4. temperatureunder heat
  5. washthe solids washed throughly with 100 ml
  6. temperatureThe combined filtrates are cooled

出典と根拠

ORDレコード
ord-ef6b8b68f41b43c7bfc76cb2c5eba972
出典データセット
uspto-grants-1978_04
特許番号
US04083997

反応ノート

読み込み中…