Sodium Hydroxide → HCID 23371888, 화합물

HRID 1900053노트

반응식

HRID 1900053 반응식
O1[C:5]2([CH2:10][CH2:9][CH:8]([C:11]3[CH:12]=[CH:13][C:14]([N:17]4[CH2:21][CH:20]([CH2:22][O:23][CH3:24])[O:19][C:18]4=[O:25])=[N:15][CH:16]=3)[CH2:7][CH2:6]2)[O:4]CC1.[OH-].[Na+]>O1CCCC1.Cl>[CH3:24][O:23][CH2:22][CH:20]1[O:19][C:18](=[O:25])[N:17]([C:14]2[CH:13]=[CH:12][C:11]([CH:8]3[CH2:9][CH2:10][C:5](=[O:4])[CH2:6][CH2:7]3)=[CH:16][N:15]=2)[CH2:21]1

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 23371867HCID 23371867, 화합물

생성물 1

HCID 23371888HCID 23371888, 화합물수율 91.6%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 0.5 g of (RS)-3-[5-(1,4-dioxa-spiro[4,5]decan-8-yl)-pyridin-2-yl]-5-methoxymethyl-oxazolidin-2-one in 20 ml of tetrahydrofuran and 5 ml of 2N hydrochloric acid was stirred at room temperature for 4 h. Then, 10 ml of 2N sodium hydroxide solution were added and the mixture was extracted several times with ethyl acetate. The organic phases were combined, dried with magnesium sulfate and concentrated. After chromatography with ethyl acetate on silica gel there was obtained 0.4 g of (RS)-5-methoxymethyl-3-[5-(4-oxo-cyclohexyl)-pyridin-2-yl]-oxazolidin-2-one. 1H-nmr (CDCl3) ppm: 8.22 (s, 1H), 8.18 (d,1H), 7.58 (d, 1H), 4.78 (m,1H), 4.27 (t, 1H), 4.09 (t, 1H), 3.64 (m, 2H), 3.43 (s, 3H), 3.08 (m, 1H), 2.51 (m, 4H), 2.04 (bm, 4H).

후처리

  1. extractionthe mixture was extracted several times with ethyl acetate
  2. dry with materialdried with magnesium sulfate
  3. concentrationconcentrated

출처 및 근거

ORD 기록
ord-dcebf407d6c14be3a73f2b43dd0e2480
출처 데이터셋
uspto-grants-1996_11
특허 번호
US05574055

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