Hydrochloric Acid → HCID 22906456, 화합물

HRID 1488781노트

반응식

HRID 1488781 반응식
[CH3:1][O:2][C:3]1[C:12]([O:13][CH3:14])=[C:11]([O:15][CH:16]([CH3:18])[CH3:17])[CH:10]=[C:9]2[C:4]=1[C:5](=[O:27])[CH:6]=[C:7]([S:19][C:20]1[CH:25]=[CH:24][C:23]([OH:26])=[CH:22][CH:21]=1)[O:8]2.C(OC([N:35](C(OC(C)(C)C)=O)[CH2:36][C:37](O)=[O:38])=O)(C)(C)C.C1(N=C=NC2CCCCC2)CCCCC1.[ClH:62]>ClCCl.C(OCC)(=O)C>[ClH:62].[CH3:1][O:2][C:3]1[C:12]([O:13][CH3:14])=[C:11]([O:15][CH:16]([CH3:18])[CH3:17])[CH:10]=[C:9]2[C:4]=1[C:5](=[O:27])[CH:6]=[C:7]([S:19][C:20]1[CH:21]=[CH:22][C:23]([O:26][C:37](=[O:38])[CH2:36][NH2:35])=[CH:24][CH:25]=1)[O:8]2

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 10868DicyclohexylcarbodiimideHCID 11509319HCID 11509319, 화합물HCID 14629457N,N-Bis(tert-butoxycarbonyl)glycine

생성물 1

HCID 22906456HCID 22906456, 화합물

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

실험 절차

300 ml in dichloromethane of 9.11 g of 5,6-dimethoxy-2-(4-hydroxyphenylthio)-7-isopropoxychromone obtained in Example 22, 4.52 g of N-t-butoxycarbonyl(Boc)glycine, and 5.32 g of dicyclohexylcarbodiimide (DCC) was stirred over 3.5 hours at room temperature. The solution thus reacted was gravitationally filtered. The solvent was distilled out from the filtrate, so that 10.95 g of N-t-butoxycarbonyl(Boc)glycine ester was obtained. 5.27 g of N-t-butoxycarbonyl(Boc)glycine ester thus prepared 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 then dried, whereby 3.53 g of 5,6-dimethoxy-2-(4-glycyloxyphenylthio)-7-isopropoxychromone 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 10.95 g of 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-74384804baea4005a81d0308f0d9c18f
출처 데이터셋
uspto-grants-1997_10
특허 번호
US05675023

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