Sodium hydride → HCID 66674083, 화합물

HRID 421810

반응식

HRID 421810 반응식
[CH:1]1([C:7]([C:9]2[CH:10]([C:27]3[CH:34]=[CH:33][C:30]([C:31]#[N:32])=[CH:29][CH:28]=3)[NH:11][C:12](=[O:26])[N:13]([C:16]3[CH:21]=[CH:20][CH:19]=[C:18]([C:22]([F:25])([F:24])[F:23])[CH:17]=3)[C:14]=2[CH3:15])=[O:8])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[H-].[Na+].Br[CH2:38][CH2:39][N:40]([CH2:43][CH3:44])[CH2:41][CH3:42]>C1COCC1>[CH:1]1([C:7]([C:9]2[CH:10]([C:27]3[CH:28]=[CH:29][C:30]([C:31]#[N:32])=[CH:33][CH:34]=3)[N:11]([CH2:38][CH2:39][N:40]([CH2:43][CH3:44])[CH2:41][CH3:42])[C:12](=[O:26])[N:13]([C:16]3[CH:21]=[CH:20][CH:19]=[C:18]([C:22]([F:25])([F:23])[F:24])[CH:17]=3)[C:14]=2[CH3:15])=[O:8])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 706082-Bromo-N,N-diethylethanamineHCID 59684783HCID 59684783, 화합물

생성물 1

HCID 66674083HCID 66674083, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a stirred solution of Example 21 (780 mg, 1.67 mmol) in THF (25 ml) is added sodium hydride (60% dispersion in mineral oil; 653 mg, 2.53 mmol). The mixture is stirred for 1 hour at room temperature, then 2-bromo-N,N-diethylethanamine (653 mg, 2.53 mmol) is added, and the solution is stirred overnight (16 h) at room temperature. The reaction mixture is quenched with methanol (10 ml), concentrated, and the crude product is purified by preparative HPLC.

후처리

  1. stirringthe solution is stirred overnight (16 h) at room temperature
  2. customThe reaction mixture is quenched with methanol (10 ml)
  3. concentrationconcentrated
  4. customthe crude product is purified by preparative HPLC

출처 및 근거

ORD 기록
ord-687052fa5a1d4a5e90cd74506f7ac943
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08101615B2

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