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Hydrochloric Acid → HCID 20478414, 화합물

HRID 904675
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HRID 904675 반응식
[Cl:1][C:2]1[C:11]2[CH:10]=[C:9]([O:12][CH3:13])[C:8]3[C:14](=[O:23])[CH:15]=[C:16]([C:18]([O:20]CC)=[O:19])[O:17][C:7]=3[C:6]=2[N:5]=[C:4]([C:24]([O:26]C)=[O:25])[CH:3]=1.Cl>C(O)(=O)C>[Cl:1][C:2]1[C:11]2[CH:10]=[C:9]([O:12][CH3:13])[C:8]3[C:14](=[O:23])[CH:15]=[C:16]([C:18]([OH:20])=[O:19])[O:17][C:7]=3[C:6]=2[N:5]=[C:4]([C:24]([OH:26])=[O:25])[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 20478384HCID 20478384, 화합물

생성물 1

HCID 20478414HCID 20478414, 화합물수율 34.5%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

To the product of step (e) (2.6 g) in glacial acetic acid (20 mls) was added concentrated hydrochloric acid (5.2 mls) and the whole was heated on a steam bath for three hours, during which time a solid slowly crystallised out of solution. The reaction mixture was cooled to room temperature and the crystallised solid was filtered off, washed thrice with glacial acetic acid and twice with diethyl ether. The resulting pale yellow solid was dried over sodium hydroxide pellets at 90° C. under a reduced pressure of 1 mm Hg for 2.5 hours, affording 0.8 g of the sub-title compound. N.M.R. Spectroscopy confirmed the structure.

후처리

  1. temperaturethe whole was heated on a steam bath for three hours, during which time a solid
  2. customslowly crystallised out of solution
  3. filtrationthe crystallised solid was filtered off
  4. washwashed thrice with glacial acetic acid
  5. dry with materialThe resulting pale yellow solid was dried over sodium hydroxide pellets at 90° C. under a reduced pressure of 1 mm Hg for 2.5 hours

출처 및 근거

ORD 기록
ord-11d7c5c63b3f414ca17b7e268f0acee7
출처 데이터셋
uspto-grants-1983_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04419352

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