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Sodium Hydroxide → HCID 19040962, 화합물

HRID 2209729
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HRID 2209729 반응식
C([O:4][C:5]1[CH:19]=[C:18]([O:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][O:26][C:27]2[CH:32]=[CH:31][C:30]([C:33]#[N:34])=[CH:29][CH:28]=2)[CH:17]=[CH:16][C:6]=1[C:7]([N:9]([CH:13]([CH3:15])[CH3:14])[CH:10]([CH3:12])[CH3:11])=[O:8])(=O)C.[OH-].[Na+]>C(O)C>[C:33]([C:30]1[CH:29]=[CH:28][C:27]([O:26][CH2:25][CH2:24][CH2:23][CH2:22][CH2:21][O:20][C:18]2[CH:17]=[CH:16][C:6]([C:7]([N:9]([CH:13]([CH3:14])[CH3:15])[CH:10]([CH3:12])[CH3:11])=[O:8])=[C:5]([OH:4])[CH:19]=2)=[CH:32][CH:31]=1)#[N:34]
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참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 15295289HCID 15295289, 화합물

생성물 1

HCID 19040962HCID 19040962, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A stirred solution of 2-acetoxy-4-[5-(4-cyanophenoxy)pentyloxy]-N,N-bis(1-methylethyl)benzamide (10 g, 21.5 mmol) in 250 mL of ethanol is treated with 1N sodium hydroxide solution (25 mL, 25 mmol). After stirring at room temperature for 2 hours, the reaction is concentrated in vacuo. This material is partitioned between ethyl acetate and 1N hydrochloric acid. The organic phase is washed with brine, dried over sodium sulfate, and concentrated in vacuo. The resulting material is purified by chromatography on silica gel (200 g) with 40-50% ethyl acetate/hexane as the eluent to afford 4-[5-(4-cyanophenoxy)pentyloxy]-2-hydroxy-N,N-bis(1-methylethyl)benzamide as a colorless foam.

후처리

  1. concentrationthe reaction is concentrated in vacuo
  2. customThis material is partitioned between ethyl acetate and 1N hydrochloric acid
  3. washThe organic phase is washed with brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe resulting material is purified by chromatography on silica gel (200 g) with 40-50% ethyl acetate/hexane as the eluent

출처 및 근거

ORD 기록
ord-1487c1d481424846b81a6c7a1c3dcc87
출처 데이터셋
uspto-grants-1995_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05455274

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