Sodium Hydroxide → 5-carboxymethyl-3-(1-carboxynonylamino)-2,3-dihydro-1,5-benzothiazepin-4(5H)-one

HRID 1719128ノート

反応式

HRID 1719128 の反応式
[C:1]([CH2:4][N:5]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[S:9][CH2:8][CH:7]([NH:16][CH:17]([C:26]([O:28]CC)=[O:27])[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])[C:6]1=[O:31])([OH:3])=[O:2].[OH-].[Na+]>C(O)C>[C:1]([CH2:4][N:5]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[S:9][CH2:8][CH:7]([NH:16][CH:17]([C:26]([OH:28])=[O:27])[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])[C:6]1=[O:31])([OH:3])=[O:2]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 134545685-carboxymethyl-3-(1-ethoxycarbonylnonylamino)-2,3-dihydro-1,5-benzothiazepin-4(5H)-one

生成物 1

HCID 202675715-carboxymethyl-3-(1-carboxynonylamino)-2,3-dihydro-1,5-benzothiazepin-4(5H)-one収率 92.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

690 mg of the 5-carboxymethyl-3-(1-ethoxycarbonylnonylamino)-2,3-dihydro-1,5-benzothiazepin-4(5H)-one obtained in Example 18 was dissolved in 10 ml of ethanol and 4 ml of a 1N aqueous solution of sodium hydroxide and then reacted at room temperature for 3 hours. After the reaction mixture was concentrated under reduced pressure, the residue was dissolved in 5 ml of water. This solution was adjusted to pH 2 with hydrochloric acid. The precipitated white crystals were separated by filtration and washed thoroughly with water to obtain 600 mg of the desired compound.

後処理

  1. concentrationAfter the reaction mixture was concentrated under reduced pressure
  2. dissolutionthe residue was dissolved in 5 ml of water
  3. customThe precipitated white crystals were separated by filtration
  4. washwashed thoroughly with water

出典と根拠

ORDレコード
ord-aae37895bee047ddbab6ed68a32fec08
出典データセット
uspto-grants-1985_09
特許番号
US04539150

反応ノート

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