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

HRID 1719118노트

반응식

HRID 1719118 반응식
C([O:3][C:4]([CH:6]([NH:15][CH:16]1[C:22](=[O:23])[N:21]([CH2:24][C:25]([O:27]CC)=[O:26])[C:20]2[CH:30]=[CH:31][CH:32]=[CH:33][C:19]=2[S:18][CH2:17]1)[CH2:7][CH2:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)=[O:5])C.[OH-].[Na+]>C(O)C>[C:4]([CH:6]([NH:15][CH:16]1[C:22](=[O:23])[N:21]([CH2:24][C:25]([OH:27])=[O:26])[C:20]2[CH:30]=[CH:31][CH:32]=[CH:33][C:19]=2[S:18][CH2:17]1)[CH2:7][CH2:8][C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1)([OH:5])=[O:3]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 134744743-(1-ethoxycarbonyl-3-phenylpropylamino)-5-ethoxycarbonylmethyl-2,3-dihydro-1,5-benzothiazepin-4(5H)-one

생성물 1

HCID 133751243-(1-carboxy-3-phenylpropylamino)-5-carboxymethyl-2,3-dihydro-1,5-benzothiazepin-4(5H)-one수율 61.5%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

1.2 g of 3-(1-ethoxycarbonyl-3-phenylpropylamino)-5-ethoxycarbonylmethyl-2,3-dihydro-1,5-benzothiazepin-4(5H)-one was dissolved in 15 ml of ethanol, and 6 ml of 1N NaOH was added thereto. The resulting mixture was stirred at room temperature, so that white crystals were precipitated. After 1.5 hours, the ethanol was distilled off under reduced pressure and water was added to the residue. After a small amount of insoluble matter was filtered off, the filtrate was adjusted to pH 3-4 with 6N hydrochloric acid. The precipitated crystals were separated by filtration and washed with cold water and then with ether to obtain 650 mg of the desired compound.

후처리

  1. customwere precipitated
  2. distillationthe ethanol was distilled off under reduced pressure and water
  3. additionwas added to the residue
  4. filtrationAfter a small amount of insoluble matter was filtered off
  5. customThe precipitated crystals were separated by filtration
  6. washwashed with cold water

출처 및 근거

ORD 기록
ord-f353b51500464d3a944c722b68f26198
출처 데이터셋
uspto-grants-1985_09
특허 번호
US04539150

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