Tert-Butylamine → HCID 10130797, 화합물

HRID 586788

반응식

HRID 586788 반응식
[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=O)=[C:4]([F:11])[CH:3]=1.[C:12]([NH2:16])([CH3:15])([CH3:14])[CH3:13].C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.Cl>C(Cl)Cl.O>[C:12]([NH:16][C:6](=[O:8])[C:5]1[CH:9]=[CH:10][C:2]([Cl:1])=[CH:3][C:4]=1[F:11])([CH3:15])([CH3:14])[CH3:13]

참가 물질

7

반응물 4

HCID 6385Tert-ButylamineHCID 757711-HydroxybenzotriazoleHCID 991524-Chloro-2-fluorobenzoic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride

생성물 1

HCID 10130797HCID 10130797, 화합물수율 96%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

To a suspension of 4-chloro-2-fluorobenzoic acid (0.3494 g, 2.00 mmol) in methylene chloride (10 ml) were added t-butylamine (0.32 ml, 3.05 mmol) and HOBt (0.3248 g, 2.40 mmol), and then WSC HCl (0.4596 g, 2.40 mmol) was added and stirred for 3 hours. The reaction mixture was added into water and extracted three times with ethyl acetate. The combined extracts were dried over MgSO4. The solvent was evaporated and the residue was purified by silica gel chromatography (hexane/ethyl acetate=5/1) to give the title compound (0.4403 g; 96%).

후처리

  1. extractionextracted three times with ethyl acetate
  2. dry with materialThe combined extracts were dried over MgSO4
  3. customThe solvent was evaporated
  4. customthe residue was purified by silica gel chromatography (hexane/ethyl acetate=5/1)

출처 및 근거

ORD 기록
ord-15e4102d01554bf98427b75ddeba1303
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06936736B2

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