Benzoyl chloride, 3-chloro- → HCID 71238641, 화합물

HRID 1846658노트

반응식

HRID 1846658 반응식
[CH2:1]([O:3][C:4](=[O:21])[CH2:5][CH:6]1[CH2:11][CH2:10][N:9]([C:12]2[C:17]([NH2:18])=[CH:16][C:15]([C:19]#[N:20])=[CH:14][N:13]=2)[CH2:8][CH2:7]1)[CH3:2].[Cl:22][C:23]1[CH:24]=[C:25]([CH:29]=[CH:30][CH:31]=1)[C:26](Cl)=[O:27]>C(#N)C>[CH2:1]([O:3][C:4](=[O:21])[CH2:5][CH:6]1[CH2:7][CH2:8][N:9]([C:12]2[C:17]([NH:18][C:26](=[O:27])[C:25]3[CH:29]=[CH:30][CH:31]=[C:23]([Cl:22])[CH:24]=3)=[CH:16][C:15]([C:19]#[N:20])=[CH:14][N:13]=2)[CH2:10][CH2:11]1)[CH3:2]

참가 물질

4

반응물 2

HCID 69252Benzoyl chloride, 3-chloro-HCID 68303889HCID 68303889, 화합물

생성물 1

HCID 71238641HCID 71238641, 화합물수율 73%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a solution of 0.043 g (0.15 mol) of (3′-amino-5′-cyano-3,4,5,6-tetrahydro-2H-[1,2′]bipyridinyl-4-yl)-acetic acid ethyl ester in acetonitrile (3 mL) is added 0.021 mL (0.16 mmol) of 3-chlorobenzoyl chloride. The mixture is stirred at room temperature for 2 hours then concentrated under reduced pressure. The residue is taken up in a saturated aqueous solution of ammonium chloride and extracted with ethyl acetate. The combined organic phase is dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue is purified by flash silica gel chromatography to give 0.047 g (73%) of [3′-(3-chloro-benzoylamino)-5′-cyano-3,4,5,6-tetrahydro-2H-[1,2′]bipyridinyl-4-yl]-acetic acid ethyl ester as a light yellow solid.

후처리

  1. concentrationthen concentrated under reduced pressure
  2. extractionextracted with ethyl acetate
  3. dry with materialThe combined organic phase is dried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue is purified by flash silica gel chromatography

출처 및 근거

ORD 기록
ord-c8505327a13d4bcfa7ead8bf20e3146f
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08952004B2

반응 노트

불러오는 중…