Hydrochloric Acid → HCID 22906475、化合物

HRID 2209658ノート

反応式

HRID 2209658 の反応式
[CH3:1][O:2][C:3]1[C:12]([O:13][CH3:14])=[C:11]([O:15][CH:16]([CH2:19][CH3:20])[CH2:17][CH3:18])[CH:10]=[C:9]2[C:4]=1[C:5](=[O:29])[CH:6]=[C:7]([S:21][C:22]1[CH:27]=[CH:26][C:25]([OH:28])=[CH:24][CH:23]=1)[O:8]2.C(OC([N:37](C(OC(C)(C)C)=O)[CH2:38][C:39](O)=[O:40])=O)(C)(C)C.C1(N=C=NC2CCCCC2)CCCCC1.[ClH:64]>ClCCl.C(OCC)(=O)C>[ClH:64].[CH2:19]([CH:16]([O:15][C:11]1[CH:10]=[C:9]2[C:4]([C:5](=[O:29])[CH:6]=[C:7]([S:21][C:22]3[CH:27]=[CH:26][C:25]([O:28][C:39](=[O:40])[CH2:38][NH2:37])=[CH:24][CH:23]=3)[O:8]2)=[C:3]([O:2][CH3:1])[C:12]=1[O:13][CH3:14])[CH2:17][CH3:18])[CH3:20]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 10868DicyclohexylcarbodiimideHCID 14629457N,N-Bis(tert-butoxycarbonyl)glycineHCID 22906525HCID 22906525、化合物

生成物 1

HCID 22906475HCID 22906475、化合物

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

300 ml in dichloromethane of 5.66 g of 5,6-dimethoxy-7-(1-ethylpropoxy)-2-(4-hydroxyphenylthio)chromone obtained in Example 25, 2.62 g of N-t-butoxycarbonyl(Boc)glycine, and 3.08 g of 1,3-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 3 hours. Subsequently, 200 ml ether was added and the resulting crystals were collected by filtration and dried, whereby 6.44 g of 7-(1-ethylpropoxy)-5,6-dimethoxy-2-(4-glycyloxyphenylthio)chromone hydrochloride with the following physicochemical properties was obtained.

後処理

  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

出典と根拠

ORDレコード
ord-06ed6fb4e25f45ed90e2e1a32b4a5d68
出典データセット
uspto-grants-1995_10
特許番号
US05455267

反応ノート

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