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Ethanol → HCID 20648927, 화합물

HRID 325247
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HRID 325247 반응식
C[O:2][C:3](=[O:31])[C:4]1[CH:9]=[CH:8][C:7]([CH2:10][N:11]2[CH:15]([CH2:16][O:17][CH:18]3[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]3)[CH2:14][CH2:13][O:12]2)=[CH:6][C:5]=1[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=1[CH3:30].[OH-].[Na+].C(O)C.P(=O)(O)(O)O>O>[CH:18]1([O:17][CH2:16][CH:15]2[CH2:14][CH2:13][O:12][N:11]2[CH2:10][C:7]2[CH:8]=[CH:9][C:4]([C:3]([OH:31])=[O:2])=[C:5]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=3[CH3:30])[CH:6]=2)[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 702EthanolHCID 1004Phosphoric AcidHCID 14798Sodium HydroxideHCID 20649182HCID 20649182, 화합물

생성물 1

HCID 20648927HCID 20648927, 화합물수율 78.5%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of example 1130C (355 mg, 0.84 mmol) and sodium hydroxide (1 mL of a 4N aqueous solution, 4 mmol) in 4 mnL of ethanol was heated to reflux for 6 hours and then cooled to room temperature. The mixture was diluted with water and the pH adjusted to 5 with aqueuos phosphoric acid. The mixture was extracted with 3 portions of ethyl acetate and the combined organic fractions were washed with water and brine, dried, filtered and concentrated to provide 270 mg (78%) of the title compound. MS (ESI+): 410 (MH+).

후처리

  1. temperatureto reflux for 6 hours
  2. extractionThe mixture was extracted with 3 portions of ethyl acetate
  3. washthe combined organic fractions were washed with water and brine
  4. customdried
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-05268e5fe38f478896ab3efe9ff3e6d6
출처 데이터셋
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06221865B1

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