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Hydrochloric Acid → 5-carboxymethyl-3-(1-ethoxycarbonylethylamino)-2,3-dihydro-1,5-benzothiazepin-4(5H)-one hydrochloride

HRID 1719122
ノート
印刷プレビュー

反応式

HRID 1719122 の反応式
C([O:5][C:6]([CH2:8][N:9]1[C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=2[S:13][CH2:12][CH:11]([NH:20][CH:21]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH3:22])[C:10]1=[O:28])=[O:7])(C)(C)C.[ClH:29]>O1CCOCC1>[ClH:29].[C:6]([CH2:8][N:9]1[C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=2[S:13][CH2:12][CH:11]([NH:20][CH:21]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH3:22])[C:10]1=[O:28])([OH:7])=[O:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 134707795-t-butoxycarbonylmethyl-3-(1-ethoxycarbonylethylamino)-2,3-dihydro-1,5-benzothiazepin-4(5H)-one

生成物 1

HCID 202675625-carboxymethyl-3-(1-ethoxycarbonylethylamino)-2,3-dihydro-1,5-benzothiazepin-4(5H)-one hydrochloride

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

0.9 g of the 5-t-butoxycarbonylmethyl-3-(1-ethoxycarbonylethylamino)-2,3-dihydro-1,5-benzothiazepin-4(5H)-one obtained in Example 11 was dissolved in 10 ml of a 6N solution of hydrogen chloride in dioxane and then reacted at room temperature for 30 minutes. After the reaction mixture was concentrated under reduced pressure, ether was added thereto so as to cause crystallization. The precipitated crystals were purified by silica gel column chromatography using a 50:3:5 mixture of chloroform, methanol and acetic acid as the eluent. Thus, there was obtained 400 mg of the desired compound.

後処理

  1. customreacted at room temperature for 30 minutes
  2. concentrationAfter the reaction mixture was concentrated under reduced pressure, ether
  3. additionwas added
  4. customcrystallization
  5. customThe precipitated crystals were purified by silica gel column chromatography
  6. additiona 50:3:5 mixture of chloroform, methanol and acetic acid as the eluent

出典と根拠

ORDレコード
ord-2331d03625bd490c8f9b50bcf336b20d
出典データセット
uspto-grants-1985_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04539150

反応ノート

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