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Hydrochloric Acid → 2-(4-Hydroxy-thianthren-1-yl)-6-morpholin-4-yl-pyran-4-one

HRID 33798
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HRID 33798 반응식
COC[O:4][C:5]1[C:18]2[S:17][C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[S:10][C:9]=2[C:8]([C:19]2[O:20][C:21]([N:26]3[CH2:31][CH2:30][O:29][CH2:28][CH2:27]3)=[CH:22][C:23](=[O:25])[CH:24]=2)=[CH:7][CH:6]=1.[I-].[Na+].Cl.[OH-].[Na+]>CC(C)=O>[OH:4][C:5]1[C:18]2[S:17][C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[S:10][C:9]=2[C:8]([C:19]2[O:20][C:21]([N:26]3[CH2:31][CH2:30][O:29][CH2:28][CH2:27]3)=[CH:22][C:23](=[O:25])[CH:24]=2)=[CH:7][CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 5238Sodium IodideHCID 14798Sodium HydroxideHCID 597974342-(4-Methoxymethoxy-thianthren-1-yl)-6-morpholin-4-yl-pyran-4-one

생성물 1

HCID 597974352-(4-Hydroxy-thianthren-1-yl)-6-morpholin-4-yl-pyran-4-one

시약·촉매·용매 1

HCID 180
Acetone
용매

실험 절차

To a solution of 2-(4-Methoxymethoxy-thianthren-1-yl)-6-morpholin-4-yl-pyran-4-one (1.1 g, 2.42 mmol) in acetone (50 ml) was added sodium iodide (0.40 g, 2.66 mmol) and concentrated HCl (3 ml). The dark suspension was stirred at room temperature for 72 hours before the careful addition of 1M sodium hydroxide solution until pH 12 was attained. The mixture was washed with EtOAc (2×50 ml) and then acidified with concentrated HCl until pH 1 whereupon a brown precipitate formed which was filtered off (0.90 g, 90%) and corresponded to the title compound. m/z (LC-MS, ESP): RT=4.39 min, (M++1)=456

후처리

  1. washThe mixture was washed with EtOAc (2×50 ml)
  2. customformed which
  3. filtrationwas filtered off (0.90 g, 90%)

출처 및 근거

ORD 기록
ord-347c25ab193b4ff6b3553ad8daa00ef9
출처 데이터셋
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07429660B2

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