Acetic Anhydride → HCID 67766488, 화합물

HRID 1898868노트

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HRID 1898868 반응식
[OH:1][C@H:2]1[C:8](=[O:9])[NH:7][C:6]2[CH:10]=[CH:11][CH:12]=[CH:13][C:5]=2[S:4][C@H:3]1[C:14]1[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=1.Cl.[CH3:23][CH:24]([CH2:27][N:28]([CH3:30])[CH3:29])[CH2:25]Cl.[C:31]([O-:34])([O-:33])=O.[K+].[K+].[C:37]([O:40][C:41](=[O:43])[CH3:42])(=[O:39])C>CC(C)=O.O.C(OCC)C>[C:37]([OH:40])(=[O:39])[C:31]([OH:34])=[O:33].[C:41]([O:1][C@H:2]1[C:8](=[O:9])[N:7]([CH2:23][CH:24]([CH3:25])[CH2:27][N:28]([CH3:30])[CH3:29])[C:6]2[CH:10]=[CH:11][CH:12]=[CH:13][C:5]=2[S:4][C@H:3]1[C:14]1[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=1)(=[O:43])[CH3:42]

참가 물질

8

반응물 4

HCID 7918Acetic AnhydrideHCID 11430Potassium CarbonateHCID 27336733-Hydroxy-2-(4-methoxyphenyl)-2,3-dihydro-1,5-benzothiazepin-4(5H)-one, (2S,3S)-HCID 30838413-Chloro-2-methylpropyl(dimethyl)ammonium chloride

생성물 1

HCID 67766488HCID 67766488, 화합물

시약·촉매·용매 3

HCID 180Acetone용매HCID 962Water용매2회HCID 3283Diethyl Ether용매

실험 절차

5 g cis(+)-2,3-dihydro-3-hydroxy-2-(4-methoxyphenyl)-1,5-benzothiazepin-4(5H)-one, 2.9 g 2-methyl-3-dimethylaminopropylchloride hydrochloride, 5.7 g K2CO3, 1.4 ml H2O were reacted in 75 ml acetone, according to the procedure as in Example 1 (a), then reacted with 70 ml acetic anhydride, (see Example 1 (b)). The crude was treated with ethyl ether and the so obtained solid is filtered off and the solution was evaporated to dryness. This procedure was repeated. 4.3 g residue were dissolved in isopropyl alcohol and treated with 1.2 g oxalic acid. A solid, which was crystallized from acetone-ethyl ether, was obtained; m.p. 84°-89° C.; [α]D20 =119.3 (H2O).

후처리

  1. filtrationthe so obtained solid is filtered off
  2. customthe solution was evaporated to dryness
  3. dissolution4.3 g residue were dissolved in isopropyl alcohol
  4. additiontreated with 1.2 g oxalic acid
  5. customA solid, which was crystallized from acetone-ethyl ether
  6. customwas obtained

출처 및 근거

ORD 기록
ord-7abc385881fd403f9078ae19bdeb4acf
출처 데이터셋
uspto-grants-1996_11
특허 번호
US05571807

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