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

HRID 1719118ノート

反応式

HRID 1719118 の反応式
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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f353b51500464d3a944c722b68f26198
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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