1,2-Dichloroethane → HCID 58333428, 화합물

HRID 2066850노트

반응식

HRID 2066850 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].[CH3:32]OC(=O)CN.C1C=C[C:41]2[N:46](O)N=[N:44][C:42]=2C=1.C(Cl)CCl>C(Cl)Cl>[CH:1]([O:4][C:5]([N:7]1[CH2:8][CH2:9][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:46][CH2:41][CH2:42][NH:44][CH3:32])=[CH:23][C:22]=3[F:31])[CH2:19][CH2:20]2)[CH2:11][CH2:12]1)=[O:6])([CH3:2])[CH3:3]

참가 물질

6

반응물 4

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

생성물 1

HCID 58333428HCID 58333428, 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 1 mL of DCM. 1 mL of TFA was added and the mixture was stirred at room temperature for 1 h. It was then concentrated under a stream of nitrogen and purified on preparative HPLC to give 31-1: LC-MS 496.5 (MH).

후처리

  1. stirringthe mixture was stirred for 18 h
  2. washThe solution was washed with 2 mL of aqueous NaHCO3
  3. concentrationconcentrated
  4. addition1 mL of TFA was added
  5. stirringthe mixture was stirred at room temperature for 1 h
  6. concentrationIt was then concentrated under a stream of nitrogen
  7. custompurified on preparative HPLC
  8. customto give 31-1

출처 및 근거

ORD 기록
ord-aad03f2391444b89879c616189bea6c2
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08293729B2

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