1,2-Dichloroethane → HCID 10133751, 화합물

HRID 352331노트

반응식

HRID 352331 반응식
C(N(CC)CC)C.Cl.[CH3:9][O:10][C:11](=[O:18])[C@H:12]([CH2:14][CH:15]([CH3:17])[CH3:16])[NH2:13].[CH:19]1[C:32]2[NH:31][C:30]3[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=3)[S:24][C:23]=2[CH:22]=[CH:21][C:20]=1[C:33](O)=[O:34].C1C=CC2N(O)N=NC=2C=1.C(Cl)CCl>CN(C=O)C>[CH3:16][CH:15]([CH3:17])[CH2:14][C@H:12]([NH:13][C:33]([C:20]1[CH:21]=[CH:22][C:23]2[S:24][C:25]3[C:30](=[CH:29][CH:28]=[CH:27][CH:26]=3)[NH:31][C:32]=2[CH:19]=1)=[O:34])[C:11]([O:10][CH3:9])=[O:18]

참가 물질

7

반응물 5

HCID 111,2-DichloroethaneHCID 8471TriethylamineHCID 757711-HydroxybenzotriazoleHCID 2723695Leucine methyl ester hydrochlorideHCID 2271159310H-Phenothiazine-2-carboxylic acid

생성물 1

HCID 10133751HCID 10133751, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

4.6 ml (33 mmoles) of triethylamine is added to a solution of 1.82 g (10 mmoles) of L-Leucine methyl ester hydrochloride, 2.43 g (10 mmoles) of 10H-phenothiazine-2-carboxylic acid (J. Med. Chem.(1998) 41 (2), 148-156), 1.48 g (11 mmoles) of HOBT and 4.21 g (22 mmoles) of EDC in 30 ml of anhydrous DMF. The reaction mixture is stirred for 15 hours. After evaporation of the solvent under vacuum, the residue is divided between 100 ml of AcOEt and 50 ml of a 1M solution of HCl. The organic phase is decanted and washed successively with 50 ml of H2O, 50 ml of a saturated solution of NaHCO3 and 50 ml of salt water. The organic solution is dried over magnesium sulphate, filtered and concentrated to dryness under vacuum. The evaporation residue is taken up in Et2O and filtered. Yellow powder (71%). Melting point: 160.5-161° C.

후처리

  1. customAfter evaporation of the solvent under vacuum
  2. customThe organic phase is decanted
  3. washwashed successively with 50 ml of H2O, 50 ml of a saturated solution of NaHCO3 and 50 ml of salt water
  4. dry with materialThe organic solution is dried over magnesium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated to dryness under vacuum
  7. filtrationfiltered

출처 및 근거

ORD 기록
ord-f86127e176fd40988b0116cb87a53115
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06747024B1

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