2,3-Dichlorobenzoic acid → HCID 66676957, 화합물

HRID 421991

반응식

HRID 421991 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 66676957HCID 66676957, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-383027df1df34715a8ea125cd65e622a
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08101621B2

연결된 노트

불러오는 중…