1,2-Dichloroethane → HCID 69289064, 화합물

HRID 2211835노트

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HRID 2211835 반응식
[C:1]([O:5][C:6]([NH:8][C@H:9]([CH2:14][C:15]1[CH:20]=[C:19]([F:21])[CH:18]=[CH:17][C:16]=1[F:22])[CH2:10][C:11]([OH:13])=O)=[O:7])([CH3:4])([CH3:3])[CH3:2].C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1.Cl.[CH3:38][N:39]1[CH2:45][CH2:44][CH2:43][NH:42][CH2:41][C:40]1=[O:46]>ClCCl.C(N(CC)CC)C>[C:1]([O:5][C:6]([NH:8][C@H:9]([CH2:14][C:15]1[CH:20]=[C:19]([F:21])[CH:18]=[CH:17][C:16]=1[F:22])[CH2:10][C:11]([N:42]1[CH2:43][CH2:44][CH2:45][N:39]([CH3:38])[C:40](=[O:46])[CH2:41]1)=[O:13])=[O:7])([CH3:2])([CH3:3])[CH3:4]

참가 물질

7

반응물 4

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 11347588(R)-b-(Boc-amino)-2,5-difluorobenzenebutanoic acidHCID 219620931-Methyl-1,4-diazepan-2-one hydrochloride

생성물 1

HCID 69289064HCID 69289064, 화합물

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8471Triethylamine용매

실험 절차

To a stirred mixture of (3R)-3-[(tert-butoxycarbonyl)amino]-4-(2,5-difluorophenyl)butanoic acid (40 mg), EDC (29 mg), and HOBT (21 mg) in dichloromethane was added triethylamine (0.042 mL) and hexahydro-1-methyl-2H-1,4-diazepin-2-one hydrochloride (33 mg). The resultant mixture was stirred at ambient temperature overnight and then concentrated. The residue was purified by preparative TLC (silica gel, 8% 10:1 methanol/concentrated ammonium hydroxide in dichloromethane) to yield the title compound.

후처리

  1. concentrationconcentrated
  2. customThe residue was purified by preparative TLC (silica gel, 8% 10:1 methanol/concentrated ammonium hydroxide in dichloromethane)

출처 및 근거

ORD 기록
ord-0b6065ec453e4389a85dd36e297e9ebb
출처 데이터셋
uspto-grants-2006_09
특허 번호
US07101871B2

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