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

HRID 1719122
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HRID 1719122 반응식
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]
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참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2331d03625bd490c8f9b50bcf336b20d
출처 데이터셋
uspto-grants-1985_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04539150

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