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Hydrochloric Acid → HCID 19040952、化合物

HRID 1683824
ノート
印刷プレビュー

反応式

HRID 1683824 の反応式
C(C1C=C[C:6]([O:7]CCCCCOC2C=CC(C(N(C(C)C)C(C)C)=O)=C(O)C=2)=[CH:5]C=1)#N.[H-].[Na+].BrCC(OCC)=O.[C:41]([C:43]1[CH:77]=[CH:76][C:46]([O:47][CH2:48][CH2:49][CH2:50][CH2:51][CH2:52][O:53][C:54]2[CH:55]=[CH:56][C:57]([C:67]([N:69]([CH:73]([CH3:75])[CH3:74])[CH:70]([CH3:72])[CH3:71])=[O:68])=[C:58]([CH:66]=2)[O:59][CH2:60][C:61]([O:63][CH2:64][CH3:65])=[O:62])=[CH:45][CH:44]=1)#[N:42].[ClH:78]>CN(C)C=O.C(O)C>[ClH:78].[CH2:64]([O:63][C:61]([CH2:60][O:59][C:58]1[CH:66]=[C:54]([CH:55]=[CH:56][C:57]=1[C:67]([N:69]([CH:73]([CH3:75])[CH3:74])[CH:70]([CH3:71])[CH3:72])=[O:68])[O:53][CH2:52][CH2:51][CH2:50][CH2:49][CH2:48][O:47][C:46]1[CH:45]=[CH:44][C:43]([C:41](=[NH:42])[O:7][CH2:6][CH3:5])=[CH:77][CH:76]=1)=[O:62])[CH3:65]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 7748Ethyl bromoacetateHCID 24758Sodium hydrideHCID 19040962HCID 19040962、化合物HCID 19040982HCID 19040982、化合物

生成物 1

HCID 19040952HCID 19040952、化合物

試薬・触媒・溶媒 2

HCID 702
Ethanol
溶媒
HCID 6228Dimethylformamide溶媒

反応条件

温度
70 °C

実験手順

A stirred solution of 4-[5-(4-cyanophenoxy)pentyloxy]-2-hydroxy-N,N-bis(1-methylethyl)benzamide (0.5 g, 1.18 mmol) in 10.0 mL of N,N-dimethylformamide is treated with 60% sodium hydride (47 mg, 1.18 mmol) and ethyl bromoacetate (144 μL, 1.3 mmol), and heated at 70° C. for 2.5 hours. The reaction is partitioned between ethyl acetate and water, dried over sodium sulfate and concentrated in vacuo to afford yellow foam. The resulting ethyl 5-[5-(4-cyanophenoxy)pentyloxy]-2-[N,N-bis(1-methylethyl)aminocarbonyl]phenoxyacetate in 50 mL of anhydrous ethanol at 0° C. is treated with anhydrous hydrogen chloride gas over 30 minutes. This solution is stirred at room temperature for 20 hours and concentrated in vacuo. This material is purified by chromatography on silica gel with 60% ethyl acetate/hexane as the eluent to afford ethyl 4-[5-[3-ethoxycarbonylmethoxy-4-[N,N-bis(1- methylethyl)aminocarbonyl]phenoxy]pentyloxy]benzenecarboximidoate monohydrochloride as colorless foam.

後処理

  1. customThe reaction is partitioned between ethyl acetate and water
  2. dry with materialdried over sodium sulfate
  3. concentrationconcentrated in vacuo
  4. customto afford yellow foam
  5. concentrationconcentrated in vacuo
  6. customThis material is purified by chromatography on silica gel with 60% ethyl acetate/hexane as the eluent

出典と根拠

ORDレコード
ord-64d84778796846c79f5e43ef4b477f67
出典データセット
uspto-grants-1997_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05639768

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート