Hydrochloric Acid → HCID 22906532, 화합물

HRID 2209657노트

반응식

HRID 2209657 반응식
[CH2:1]([O:3][C:4]1[C:13]([O:14][CH3:15])=[C:12]([O:16][CH:17]([CH3:19])[CH3:18])[CH:11]=[C:10]2[C:5]=1[C:6](=[O:28])[CH:7]=[C:8]([S:20][C:21]1[CH:26]=[CH:25][C:24]([OH:27])=[CH:23][CH:22]=1)[O:9]2)[CH3:2].C(OC([N:36](C(OC(C)(C)C)=O)[CH2:37][C:38](O)=[O:39])=O)(C)(C)C.C1(N=C=NC2CCCCC2)CCCCC1.[ClH:63]>ClCCl.C(OCC)(=O)C>[ClH:63].[CH2:1]([O:3][C:4]1[C:13]([O:14][CH3:15])=[C:12]([O:16][CH:17]([CH3:19])[CH3:18])[CH:11]=[C:10]2[C:5]=1[C:6](=[O:28])[CH:7]=[C:8]([S:20][C:21]1[CH:26]=[CH:25][C:24]([O:27][C:38](=[O:39])[CH2:37][NH2:36])=[CH:23][CH:22]=1)[O:9]2)[CH3:2]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 10868DicyclohexylcarbodiimideHCID 14629457N,N-Bis(tert-butoxycarbonyl)glycineHCID 15288794HCID 15288794, 화합물

생성물 1

HCID 22906532HCID 22906532, 화합물

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

실험 절차

300 ml in dichloromethane of 11.35 g of 5-ethoxy-2-(4-hydroxyphenylthio)-7-isopropoxy-6-methoxychromone obtained in Example 18, 5.43 g of N-t-butoxycarbonyl(Boc)glycine, and 6.40 g of dicyclohexylcarbodiimide (DCC) was stirred over 5.5 hours at room temperature. The solution thus reacted was gravitationally filtered. The solvent was distilled out from the filtrate, so that N-t-butoxycarbonyl(Boc)glycine ester was obtained. This product was dissolved in 100 ml of ethyl acetate. Then, hydrochloric acid gas was introduced and bubbled in the solution for 10 min., followed by stirring for 1 hour. Subsequently, 200 ml ether was added and the resulting crystals were collected by filtration and dried, whereby 11.28 g of 5-ethoxy-2-(4-glycyloxyphenylthio)-7-isopropoxy-6-methoxychromone hydrochloride with the following physicochemical properties was obtained.

후처리

  1. customThe solution thus reacted
  2. filtrationwas gravitationally filtered
  3. distillationThe solvent was distilled out from the filtrate, so that N-t-butoxycarbonyl(Boc)glycine ester
  4. customwas obtained
  5. custombubbled in the solution for 10 min.
  6. additionSubsequently, 200 ml ether was added
  7. filtrationthe resulting crystals were collected by filtration
  8. customdried

출처 및 근거

ORD 기록
ord-0de68d68f0ba40eb9b10de08fa5fb46a
출처 데이터셋
uspto-grants-1995_10
특허 번호
US05455267

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