Ammonia → HCID 57194161、化合物

HRID 1901169

反応式

HRID 1901169 の反応式
C[O:2][C:3]([CH2:5][C:6]1[CH:26]=[CH:25][C:9]([O:10][CH2:11][CH:12]([NH:14][CH2:15][CH:16]([C:18]2[CH:23]=[CH:22][CH:21]=[C:20]([Cl:24])[CH:19]=2)[OH:17])[CH3:13])=[C:8]([Cl:27])[CH:7]=1)=O.[NH3:28]>CO>[C:3]([CH2:5][C:6]1[CH:26]=[CH:25][C:9]([O:10][CH2:11][CH:12]([NH:14][CH2:15][CH:16]([C:18]2[CH:23]=[CH:22][CH:21]=[C:20]([Cl:24])[CH:19]=2)[OH:17])[CH3:13])=[C:8]([Cl:27])[CH:7]=1)(=[O:2])[NH2:28]

参加物

4

反応物 2

HCID 222AmmoniaHCID 218321762-[2-(4-Methoxycarbonylmethyl-2-chlorophenoxy)-1-methylethyl]amino-1-(3-chlorophenyl)ethanol

生成物 1

HCID 57194161HCID 57194161、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 2 g of 2-[2-(4-methoxycarbonylmethyl-2-chlorophenoxy) -1-methylethyl]amino-1-(3-chlorophenyl)ethanol (prepared as described in Example 22) dissolved in 50 ml of methanol was saturated with gaseous ammonia in a reaction vessel, whilst ice-cooling, after which the reaction vessel was tightly stoppered and allowed to stand at room temperature for one week. At the end of this time, the solvent (methanol) was removed by distillation under reduced pressure, and the residue was recrystallized from ethyl acetate, to give 0.55 g of the title compound as crystals, melting at 99°-101° C.

後処理

  1. temperaturecooling
  2. waitto stand at room temperature for one week
  3. customAt the end of this time, the solvent (methanol) was removed by distillation under reduced pressure
  4. customthe residue was recrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-c4979ee582e84021838b5db0b01330d9
出典データセット
uspto-grants-1996_11
特許番号
US05576340

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