Chloride → 1,10-Bis(3',5'-dimethyl-4'-hydroxyphenylcarbonyl)-1,10-diaza-4,7,13,16-tetraoxacyclooctadecane

HRID 2288252ノート

反応式

HRID 2288252 の反応式
[Cl-].[CH3:2][C:3]1[CH:4]=[C:5]([C:14]([N:16]2[CH2:33][CH2:32][O:31][CH2:30][CH2:29][O:28][CH2:27][CH2:26][N:25]([C:34]([C:36]3[CH:41]=[C:40]([CH3:42])[C:39]([O:43]C(=O)C)=[C:38]([CH3:47])[CH:37]=3)=[O:35])[CH2:24][CH2:23][O:22][CH2:21][CH2:20][O:19][CH2:18][CH2:17]2)=[O:15])[CH:6]=[C:7]([CH3:13])[C:8]=1[O:9]C(=O)C.C[O-].[Na+]>CO>[CH3:13][C:7]1[CH:6]=[C:5]([C:14]([N:16]2[CH2:33][CH2:32][O:31][CH2:30][CH2:29][O:28][CH2:27][CH2:26][N:25]([C:34]([C:36]3[CH:41]=[C:40]([CH3:42])[C:39]([OH:43])=[C:38]([CH3:47])[CH:37]=3)=[O:35])[CH2:24][CH2:23][O:22][CH2:21][CH2:20][O:19][CH2:18][CH2:17]2)=[O:15])[CH:4]=[C:3]([CH3:2])[C:8]=1[OH:9]

参加物

5

反応物 3

HCID 312ChlorideHCID 10942334Sodium MethoxideHCID 187041651,10-Bis(3',5'-dimethyl-4'-acetoxyphenylcarbonyl)-1,10-diaza-4,7,13,16-tetraoxacyclooctadecane

生成物 1

HCID 187041871,10-Bis(3',5'-dimethyl-4'-hydroxyphenylcarbonyl)-1,10-diaza-4,7,13,16-tetraoxacyclooctadecane収率 89.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
0 °C

実験手順

To 40 ml of mixed solvent of anhydrous methanolmethylene chloride was dissolved 0.5 g/0.8 mmol of 1,10-bis(3',5'-dimethyl-4'-acetoxyphenylcarbonyl)-1,10-diaza-4,7,13,16-tetraoxacyclooctadecane, and the solution was cooled to 0° C. To this solution was added 2.6 ml of freshly prepared 1M methanol solution of sodium methoxide, and the mixture was stirred at 0° C. for 2 hours. After adding Amberlite 15 until the reaction solution became neutral, the resin was separated by filtration and the filtrate was concentrated under reduced pressure to obtain 0.4 g of 1,10-bis(3',5'-dimethyl-4'-hydroxyphenylcarbonyl)-1,10-diaza-4,7,13,16-tetraoxacyclooctadecane. 1H-NMR (CDCl3): δ2.15 (12H, s), 3.6 (16H, br), 3.8 (8H, br), 5.89 (2H, s), 6.90 (4H, s).

後処理

  1. additionAfter adding Amberlite 15 until the reaction solution
  2. customthe resin was separated by filtration
  3. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-0a4dbd4e19074b6b8e0164b1b9069a4b
出典データセット
uspto-grants-2000_07
特許番号
US06087502

反応ノート

読み込み中…