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Carbon tetrabromide → HCID 67341717, 화합물

HRID 1846616
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HRID 1846616 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:25]=[CH:26][CH:27]=1)[C:5]([NH:7][C:8]1[C:9]([N:15]2[CH2:20][CH2:19][CH:18]([CH2:21][CH2:22][CH2:23]O)[CH2:17][CH2:16]2)=[N:10][CH:11]=[C:12]([Cl:14])[CH:13]=1)=[O:6].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Br)(Br)(Br)[Br:48]>C(Cl)Cl>[Br:48][CH2:23][CH2:22][CH2:21][CH:18]1[CH2:19][CH2:20][N:15]([C:9]2[C:8]([NH:7][C:5](=[O:6])[C:4]3[CH:25]=[CH:26][CH:27]=[C:2]([Cl:1])[CH:3]=3)=[CH:13][C:12]([Cl:14])=[CH:11][N:10]=2)[CH2:16][CH2:17]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11205Carbon tetrabromideHCID 11776TriphenylphosphineHCID 67341654HCID 67341654, 화합물

생성물 1

HCID 67341717HCID 67341717, 화합물수율 40%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of 0.080 g (0.20 mmol) of the above amide and 0.056 g (0.22 mmol) of triphenylphosphine in anhydrous methylene chloride (10 mL), under an atmosphere of nitrogen, is stirred at room temperature for 20 minutes. To this mixture is added 0.071 g (0.22 mmol) of carbon tetrabromide and the resulting mixture is stirred overnight at room temperature. The reaction mixture is concentrated under reduced pressure and the residue is purified by flash silica gel chromatography to give 0.037 g (40%) of N-[4-(3-bromo-propyl)-5′-chloro-3,4,5,6-tetrahydro-2H-[1,2′]bipyridinyl-3′-yl]-3-chloro-benzamide.

후처리

  1. stirringthe resulting mixture is stirred overnight at room temperature
  2. concentrationThe reaction mixture is concentrated under reduced pressure
  3. customthe residue is purified by flash silica gel chromatography

출처 및 근거

ORD 기록
ord-6e6ca26266c34cf78f728bf1c2c50e5d
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08952004B2

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