1-Hydroxybenzotriazole hydrate → HCID 178471441、化合物

HRID 1666985ノート

反応式

HRID 1666985 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

HCID 178471441HCID 178471441、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8d0d55b287094850bb061693dc26f62a
出典データセット
uspto-grants-2011_10
特許番号
US08044208B2

反応ノート

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