Acetic Acid → HCID 13066647、化合物

HRID 1606635ノート

反応式

HRID 1606635 の反応式
C([O:4][C:5]1[CH:36]=[CH:35][CH:34]=[CH:33][C:6]=1[C:7]([NH:9][C:10]1[CH:19]=[CH:18][C:17]([NH:20][C:21](=[O:32])[C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=2[O:28]C(=O)C)=[CH:16][C:11]=1[C:12]([O:14][CH3:15])=[O:13])=[O:8])(=O)C.C(=O)([O-])[O-].[Na+].[Na+].C(O)(=O)C>CO.O>[C:7]([NH:9][C:10]1[CH:19]=[CH:18][C:17]([NH:20][C:21](=[O:32])[C:22]2[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=2)[OH:28])=[CH:16][C:11]=1[C:12]([O:14][CH3:15])=[O:13])(=[O:8])[C:6]1[C:5](=[CH:36][CH:35]=[CH:34][CH:33]=1)[OH:4]

参加物

6

反応物 3

HCID 176Acetic AcidHCID 10340Sodium CarbonateHCID 13066645HCID 13066645、化合物

生成物 1

HCID 13066647HCID 13066647、化合物収率 86.5%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒2 回

実験手順

In 150 ml methanol was dissolved 5.3 g of methyl 2,5-bis(2'-acetoxybenzamido)-benzoate obtained in Example 3. To the solution was added 2.5 g of sodium carbonate dissolved in 40 ml of water and then the mixture was stirred at room temperature for 30 minutes. The mixture was poured into 500 ml of water containing 10 ml of acetic acid to precipitate crystals. The crystals were recovered by filtration, washed with water, dried and recrystallized from ethyl acetate to yield 3.8 g of methyl 2,5-bis(salicylamido)-benzoate having a melting point between 243° - 244°C.

後処理

  1. customto precipitate crystals
  2. filtrationThe crystals were recovered by filtration
  3. washwashed with water
  4. customdried
  5. customrecrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-a47513806b9f477b85e94148d2e689d5
出典データセット
uspto-grants-1976_04
特許番号
US03953496

反応ノート

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