1,2-Dichloroethane → HCID 58333591, 화합물

HRID 2066849노트

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HRID 2066849 반응식
[CH:1]([O:4][C:5]([N:7]1[CH2:12][CH2:11][CH:10]([O:13][N:14]=[C:15]2[CH2:20][CH2:19][N:18]([C:21]3[CH:26]=[C:25]([F:27])[C:24]([C:28](O)=[O:29])=[CH:23][C:22]=3[F:31])[CH2:17][CH2:16]2)[CH2:9][CH2:8]1)=[O:6])([CH3:3])[CH3:2].C[O:33][C:34](=[O:37])[CH2:35][NH2:36].C1C=CC2N(O)N=NC=2C=1.C(Cl)CCl>C(Cl)Cl>[CH:1]([O:4][C:5]([N:7]1[CH2:12][CH2:11][CH:10]([O:13][N:14]=[C:15]2[CH2:16][CH2:17][N:18]([C:21]3[CH:26]=[C:25]([F:27])[C:24]([C:28](=[O:29])[NH:36][CH2:35][C:34]([OH:33])=[O:37])=[CH:23][C:22]=3[F:31])[CH2:19][CH2:20]2)[CH2:9][CH2:8]1)=[O:6])([CH3:3])[CH3:2]

참가 물질

6

반응물 4

HCID 111,2-DichloroethaneHCID 69221Glycine methyl esterHCID 757711-HydroxybenzotriazoleHCID 58333593HCID 58333593, 화합물

생성물 1

HCID 58333591HCID 58333591, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

9-1 (32 mg, 0.073 mmol), amino-acetic acid methyl ester (0.11 mmol) and HOBT (15 mg, 0.11 mmol) were combined in DCM (1 mL) and stirred at room temperature for 10 minutes. EDC(19 mg, 0.1 mmol) was added and the mixture was stirred for 18 h. The solution was washed with 2 mL of aqueous NaHCO3, concentrated and taken up with 0.5 mL of dioxane. 0.5 mL of 1N NaOH was added and the mixture was stirred at 60° C. for 1 h. It was then cooled to room temperature, acidified with 0.5 mL of 2N HCl and extracted with ethyl acetate (1.5 mL). The organic layer was concentrated under a stream of nitrogen and purified on preparative HPLC to give 30-1: LC-MS 497.4 (MH).

후처리

  1. stirringthe mixture was stirred for 18 h
  2. washThe solution was washed with 2 mL of aqueous NaHCO3
  3. concentrationconcentrated
  4. addition0.5 mL of 1N NaOH was added
  5. stirringthe mixture was stirred at 60° C. for 1 h
  6. temperatureIt was then cooled to room temperature
  7. extractionextracted with ethyl acetate (1.5 mL)
  8. concentrationThe organic layer was concentrated under a stream of nitrogen
  9. custompurified on preparative HPLC
  10. customto give 30-1

출처 및 근거

ORD 기록
ord-f9ce94e424654746bb5bbb383a37d5e8
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08293729B2

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