Dibromoacetic Acid → HCID 89613707、化合物

HRID 623284

反応式

HRID 623284 の反応式
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]

参加物

6

反応物 3

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

生成物 1

HCID 89613707HCID 89613707、化合物収率 15%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒2 回

実験手順

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%)

後処理

  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%)

出典と根拠

ORDレコード
ord-ffdd7d0ce13447fcab851325e1354a4c
出典データセット
uspto-grants-2016_04
特許番号
US09301525B2

関連ノート

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