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

HRID 1719128노트

반응식

HRID 1719128 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-aae37895bee047ddbab6ed68a32fec08
출처 데이터셋
uspto-grants-1985_09
특허 번호
US04539150

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