Hydrochloric Acid → HCID 25189985, 화합물

HRID 1517498노트

반응식

HRID 1517498 반응식
[CH3:1][C:2]12[C:14]3[C:6](=[CH:7][C:8]([NH:15][C:16]([C:18]4[CH:27]=[CH:26][C:21]([C:22]([O:24]C)=[O:23])=[CH:20][N:19]=4)=[O:17])=[CH:9][C:10]=3[CH2:11][CH2:12][CH2:13]1)[CH2:5][CH2:4][CH2:3]2.[OH-].[Na+].Cl>C(O)C>[CH3:1][C:2]12[C:14]3[C:6](=[CH:7][C:8]([NH:15][C:16]([C:18]4[CH:27]=[CH:26][C:21]([C:22]([OH:24])=[O:23])=[CH:20][N:19]=4)=[O:17])=[CH:9][C:10]=3[CH2:11][CH2:12][CH2:13]1)[CH2:5][CH2:4][CH2:3]2

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 25189986HCID 25189986, 화합물

생성물 1

HCID 25189985HCID 25189985, 화합물수율 91%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A suspension of methyl 6-[(6a-methyl-5,6,6a,7,8,9-hexahydro-4H-2-phenalenyl)carbamoyl]nicotinate (0.176 g) in ethanol (10 ml) was added with 2 N aqueous sodium hydroxide (2 ml), and the mixture was stirred at room temperature for 3 hours. The reaction mixture was made acidic with 2 N aqueous hydrochloric acid, and the mixture was extracted with chloroform. The organic layer was washed with saturated brine, and dried over anhydrous sodium sulfate. The organic layer was concentrated under reduced pressure, and the resulting residue was recrystallized from ethyl acetate-n-hexane to obtain the title compound (0.153 g, yield: 91%) as pale yellow needles (melting point: 212-213° C.).

후처리

  1. extractionthe mixture was extracted with chloroform
  2. washThe organic layer was washed with saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationThe organic layer was concentrated under reduced pressure
  5. customthe resulting residue was recrystallized from ethyl acetate-n-hexane

출처 및 근거

ORD 기록
ord-ece2e1e9a3364b20bf9125b7d0fdcd98
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08232300B2

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