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1,2-Dichloroethane → HCID 131725244, 화합물

HRID 489689
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HRID 489689 반응식
CO[CH:3](OC)[CH2:4][NH:5][C:6]([NH:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[CH:15]1[CH2:20][CH2:19][N:18]([C:21]([O:23]C(C)(C)C)=O)[CH2:17][CH2:16]1)=[O:7].C(O)(C(F)(F)F)=O.[NH:37]([C:50]([O:52][C:53]([CH3:56])([CH3:55])[CH3:54])=[O:51])[C@@H:38](C(O)=O)[CH2:39][C:40]1[CH:45]=[CH:44][C:43]([Cl:46])=[CH:42][CH:41]=1.C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1>C(Cl)Cl>[Cl:46][C:43]1[CH:42]=[CH:41][C:40]([CH2:39][C@@H:38]([NH:37][C:50]([O:52][C:53]([CH3:56])([CH3:55])[CH3:54])=[O:51])[C:21](=[O:23])[N:18]2[CH2:17][CH2:16][CH:15]([C:10]3[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=3[N:8]3[CH:3]=[CH:4][NH:5][C:6]3=[O:7])[CH2:20][CH2:19]2)=[CH:45][CH:44]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 111,2-DichloroethaneHCID 6422Trifluoroacetic acid2회HCID 757711-HydroxybenzotriazoleHCID 7018791N-Boc-4-chloro-D-phenylalanineHCID 22266258HCID 22266258, 화합물

생성물 1

HCID 131725244HCID 131725244, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

The title compound was prepared according to the procedure described in Example 17 (Step b) using tert-butyl 4-(2-{[(2,2-dimethoxyethyl)amino]carbonylamino}phenyl)piperidine-carboxylate (Step a) (0.742 g, 1.82 mmol) and a 50% aqueous TFA soln (20 mL) followed by Boc-p-Cl-D-PheOH (Advanced ChemTech) (0.545 g, 1.82 mmol), EDC (Advanced ChemTech) (0.523 g, 2.73 mmol), HOBT (Novabiochem) (0.246 g, 1.82 mmol) and TFA (Aldrich) (0.25 mL, 1.82 mmol) in CH2Cl2 (10 mL). Purification by silica gel chromatography (100% EtOAc then 1:9 MeOH:EtOAc) provided the title compound as a white solid (0.675 g). MS (ESI, pos. ion) m/z: 525 (M+1). Calc'd for C28H33ClN4O4: 524.22.

후처리

  1. customThe title compound was prepared
  2. customPurification by silica gel chromatography (100% EtOAc

출처 및 근거

ORD 기록
ord-2ff4db042ac14bd8b26fee42e2ff7da8
출처 데이터셋
uspto-grants-2005_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06977264B2

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