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Hydrochloric Acid → HCID 178420090, 화합물

HRID 2407682
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HRID 2407682 반응식
[C:1]1([C:7]2[CH:11]=[C:10]([CH2:12][N:13]3[CH2:18][CH2:17][CH:16]([CH2:19][NH:20][C:21]4[C:29]5[C:24](=[CH:25][CH:26]=[C:27]([C:30]6[N:34]=[CH:33][N:32](C(C7C=CC=CC=7)(C7C=CC=CC=7)C7C=CC=CC=7)[N:31]=6)[CH:28]=5)[N:23](C5CCCCO5)[N:22]=4)[CH2:15][CH2:14]3)[O:9][N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CO.Cl.C(=O)(O)[O-].[Na+]>O1CCCC1.O>[C:1]1([C:7]2[CH:11]=[C:10]([CH2:12][N:13]3[CH2:14][CH2:15][CH:16]([CH2:19][NH:20][C:21]4[C:29]5[C:24](=[CH:25][CH:26]=[C:27]([C:30]6[N:34]=[CH:33][NH:32][N:31]=6)[CH:28]=5)[NH:23][N:22]=4)[CH2:17][CH2:18]3)[O:9][N:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 516892Sodium BicarbonateHCID 58504049HCID 58504049, 화합물

생성물 1

HCID 178420090HCID 178420090, 화합물수율 52.9%

시약·촉매·용매 2

HCID 962Water용매
HCID 8028
Tetrahydrofuran
용매

실험 절차

The compound prepared in Example 72 (0.13 g) was suspended in a mixture of tetrahydrofuran (6 mL), methanol (6 mL), water (1.5 mL) and concentrated hydrochloric acid (1.5 mL) and heated at reflux overnight. The reaction mixture was cooled to room temperature and poured into a saturated aqueous sodium bicarbonate solution and extracted into ethyl acetate. The organics were dried over anhydrous magnesium sulfate and concentrated. The residue was purified by column chromatography on silica gel to obtain the title compound (0.040 g) having the following physical data.

후처리

  1. temperatureheated
  2. temperatureat reflux overnight
  3. extractionextracted into ethyl acetate
  4. dry with materialThe organics were dried over anhydrous magnesium sulfate
  5. concentrationconcentrated
  6. customThe residue was purified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-420e3f148f8c4f4c9522f5bb1dfbd503
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08809538B2

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