1-Hydroxybenzotriazole hydrate → HCID 178471441, 화합물

HRID 1666985노트

반응식

HRID 1666985 반응식
[C:1]([O:5][C:6]([NH:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13]([C:24]1[N:25]=[CH:26][N:27](S(C2C=CC(C)=CC=2)(=O)=O)[CH:28]=1)([C:19]([O:21][CH2:22][CH3:23])=[O:20])[C:14]([O:16][CH2:17][CH3:18])=[O:15])=[O:7])([CH3:4])([CH3:3])[CH3:2].O.ON1C2C=CC=CC=2N=N1>CO.C(OCC)(=O)C>[C:1]([O:5][C:6]([NH:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13]([C:24]1[N:25]=[CH:26][NH:27][CH:28]=1)([C:19]([O:21][CH2:22][CH3:23])=[O:20])[C:14]([O:16][CH2:17][CH3:18])=[O:15])=[O:7])([CH3:3])([CH3:4])[CH3:2]

참가 물질

5

반응물 2

HCID 27960291-Hydroxybenzotriazole hydrateHCID 67444839Diethyl 2-(4-tert-butoxycarbonylaminobutyl)-2-[1-(toluene-4-sulfonyl)-1H-imidazol-4-yl]malonate

생성물 1

HCID 178471441HCID 178471441, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 8857Ethyl Acetate용매

실험 절차

4.2 g (7.61 mmol) of diethyl 2-(4-tert-butoxycarbonylaminobutyl)-2-[1-(toluene-4-sulfonyl)-1H-imidazol-4-yl]malonate were dissolved in 190 ml of methanol and stirred with 4.66 g (30.45 mmol) of 1-hydroxybenzotriazole hydrate at RT for 1 h. The reaction mixture was concentrated under reduced pressure, and the residue was chromatographed on silica gel (CH2Cl2:MeOH 9:1). The product-containing fractions were concentrated and the oil obtained was dissolved in ethyl acetate and washed with saturated NaHCO3 solution. The organic phase was dried over Na2SO4, filtered and concentrated. This gave 2.14 g (71%) of the title compound.

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customthe residue was chromatographed on silica gel (CH2Cl2:MeOH 9:1)
  3. concentrationThe product-containing fractions were concentrated
  4. customthe oil obtained
  5. washwashed with saturated NaHCO3 solution
  6. dry with materialThe organic phase was dried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-8d0d55b287094850bb061693dc26f62a
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08044208B2

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