1,2-Dichloroethane → HCID 86754341、化合物

HRID 583707ノート

反応式

HRID 583707 の反応式
[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]

参加物

7

反応物 5

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

生成物 1

HCID 86754341HCID 86754341、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-b14848722f0d4399b5d7f3a79413d3ca
出典データセット
uspto-grants-1999_07
特許番号
US05929120

反応ノート

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