Dibromoacetic Acid → HCID 89613707, 화합물

HRID 623284

반응식

HRID 623284 반응식
Cl.[Cl:2][C:3]1[N:8]=[CH:7][C:6]([CH2:9][N:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]2=[NH:16])=[CH:5][CH:4]=1.CCN=C=NCCCN(C)C.Cl.[Br:29][CH:30]([Br:34])[C:31](O)=[O:32]>CN(C1C=CN=CC=1)C.ClCCl>[Br:29][CH:30]([Br:34])[C:31]([N:16]=[C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][N:10]1[CH2:9][C:6]1[CH:7]=[N:8][C:3]([Cl:2])=[CH:4][CH:5]=1)=[O:32]

참가 물질

6

반응물 3

HCID 12433Dibromoacetic AcidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 86686930HCID 86686930, 화합물

생성물 1

HCID 89613707HCID 89613707, 화합물수율 15%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매2회

실험 절차

200 mg (0.78 mmol) of the 1-[(6-chloropyridin-3-yl)methyl]pyridin-2(1H)-imine hydrochloride obtained by the method described in another method of Synthetic Example P1, 238 mg (1.95 mmol) of DMAP and 224 mg (1.17 mmol) of EDC-HCl were dissolved in 10 ml of anhydrous dichloromethane, 101 μl (202 mg, 1.17 mmol) of dibromoacetic acid was added thereto, and the resulting mixture was stirred at room temperature overnight. After the reaction was completed, the reaction solution was diluted with dichloromethane, washed once with water and twice with a 1% HCl aqueous solution, and then dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain the subject material. Amount obtained 50 mg (yield 15%)

후처리

  1. washwashed once with water and twice with a 1% HCl aqueous solution
  2. dry with materialdried over anhydrous magnesium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customto obtain the subject material
  5. customAmount obtained 50 mg (yield 15%)

출처 및 근거

ORD 기록
ord-ffdd7d0ce13447fcab851325e1354a4c
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09301525B2

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