1,2-Dichloroethane → HCID 86754341, 화합물

HRID 583707노트

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HRID 583707 반응식
[NH:1]1[C:9]2[C:4](=[N:5][CH:6]=[CH:7][CH:8]=2)[N:3]=[C:2]1[CH:10]=[CH:11][C:12]1[CH:20]=[CH:19][C:15]([C:16]([OH:18])=O)=[CH:14][CH:13]=1.Cl.[NH2:22][CH2:23][C@H:24]([NH:32][S:33]([C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1)(=[O:35])=[O:34])[C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26].C1C=CC2N(O)N=NC=2C=1.C(Cl)CCl.CN1CCOCC1>CN(C=O)C>[C:28]([O:27][C:25](=[O:26])[C@@H:24]([NH:32][S:33]([C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1)(=[O:35])=[O:34])[CH2:23][NH:22][C:16](=[O:18])[C:15]1[CH:14]=[CH:13][C:12]([CH:11]=[CH:10][C:2]2[NH:1][C:9]3[C:4]([N:3]=2)=[N:5][CH:6]=[CH:7][CH:8]=3)=[CH:20][CH:19]=1)([CH3:31])([CH3:29])[CH3:30]

참가 물질

7

반응물 5

HCID 111,2-DichloroethaneHCID 79724-MethylmorpholineHCID 757711-HydroxybenzotriazoleHCID 22853534(S)-3-amino-2-benzenesulfonylamino-propionic acid tert-butyl ester hydrochlorideHCID 53849864HCID 53849864, 화합물

생성물 1

HCID 86754341HCID 86754341, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A DMF solution (10 mL) containing 31-3 (301 mg, 1.0 mmol) 2-1 (336 mg, 1.0 mmol), HOBT (206 mg, 1.35 mmol), EDC (258 mg, 1.35 mmol) and NMM (440 μl, 4.0 mmol) was stirred under ambient conditions for 18 h. The DMF was evaporated and the residue partitioned between CH2Cl2 and H2O. The organic layer was dried (MgSO4) and concentrated to a yellow gum which was purified by flash chromatography (silica, 4:1, CHCl3 ·NH3 /IPA) to provide impure 31-4 which was rechromatographed (silica, 9:1 EtOAc/IPA) to give 31-4 as a colorless foam.

후처리

  1. customThe DMF was evaporated
  2. customthe residue partitioned between CH2Cl2 and H2O
  3. dry with materialThe organic layer was dried (MgSO4)
  4. concentrationconcentrated to a yellow gum which
  5. customwas purified by flash chromatography (silica, 4:1, CHCl3 ·NH3 /IPA)
  6. customto provide impure 31-4 which
  7. customwas rechromatographed (silica, 9:1 EtOAc/IPA)

출처 및 근거

ORD 기록
ord-b14848722f0d4399b5d7f3a79413d3ca
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05929120

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