2,3-Dichlorobenzoic acid → HCID 66676957、化合物

HRID 421991

反応式

HRID 421991 の反応式
[C@H:1]12[CH2:7][C@H:4]([NH:5][CH2:6]1)[CH2:3][N:2]2[C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9].ON1C2C=CC=CC=2N=N1.[Cl:25][C:26]1[C:34]([Cl:35])=[CH:33][CH:32]=[CH:31][C:27]=1[C:28](O)=[O:29]>C(Cl)(Cl)Cl>[Cl:25][C:26]1[C:34]([Cl:35])=[CH:33][CH:32]=[CH:31][C:27]=1[C:28]([N:5]1[CH2:6][C@@H:1]2[CH2:7][C@H:4]1[CH2:3][N:2]2[C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])=[O:29]

参加物

5

反応物 3

HCID 57652,3-Dichlorobenzoic acidHCID 757711-HydroxybenzotriazoleHCID 11521263(1S,4S)-2-Boc-2,5-diazabicyclo[2.2.1]heptane

生成物 1

HCID 66676957HCID 66676957、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

To a mixture of 3.0 g of tert-butyl (1S,4S)-2,5-diazabicyclo[2.2.1]heptane-2-carboxylate, 3.2 g of 1-(3-dimethyl-aminopropyl) -3-ethylcarbodiimide hydrochloride, 2.6 g of 1-hydroxybenzotriazole, 2.9 g of 2,3-dichlorobenzoic acid and 60 ml of chloroform was stirred at room temperature for 17 hours and then diluted with chloroform. An insoluble matter was filtered off using Celite and the resulting mixture was washed with water with saturated brine. The resulting organic layer was dried over magnesium sulfate and filtered, the filtrate was concentrated in vacuo and the resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate=9/1 to 1/1) to give the title compound.

後処理

  1. filtrationAn insoluble matter was filtered off
  2. washthe resulting mixture was washed with water with saturated brine
  3. dry with materialThe resulting organic layer was dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationthe filtrate was concentrated in vacuo
  6. customthe resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate=9/1 to 1/1)

出典と根拠

ORDレコード
ord-383027df1df34715a8ea125cd65e622a
出典データセット
uspto-grants-2012_01
特許番号
US08101621B2

関連ノート

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