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1,2-Dichloroethane → [2-(3-butoxy-3-o-tolyl-azetidin-1-yl)-1-(4-hydroxybenzyl)-2-oxoethyl]-3-(3H-imidazol-4-yl)propionamide

HRID 540419
ノート
印刷プレビュー

反応式

HRID 540419 の反応式
[CH2:1](Cl)[CH2:2]Cl.C1C=CC2N(O)N=[N:11]C=2C=1.C(OC(N[C@H:23]([CH2:27][C:28]1[CH:33]=[CH:32][C:31]([OH:34])=[CH:30][CH:29]=1)[C:24]([OH:26])=O)=O)(C)(C)C.FC(F)(F)C(O)=O.[CH2:42]([O:46][C:47]1([C:51]2[CH:56]=[CH:55][CH:54]=[CH:53][C:52]=2[CH3:57])[CH2:50][NH:49][CH2:48]1)[CH2:43][CH2:44][CH3:45].C([N:60]([CH2:63]C)[CH2:61][CH3:62])C.Cl.C[N:67](C)[CH:68]=[O:69]>>[CH2:42]([O:46][C:47]1([C:51]2[CH:56]=[CH:55][CH:54]=[CH:53][C:52]=2[CH3:57])[CH2:48][N:49]([C:24](=[O:26])[CH:23]([CH:1]([CH2:2][C:62]2[NH:11][CH:63]=[N:60][CH:61]=2)[C:68]([NH2:67])=[O:69])[CH2:27][C:28]2[CH:29]=[CH:30][C:31]([OH:34])=[CH:32][CH:33]=2)[CH2:50]1)[CH2:43][CH2:44][CH3:45]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 7

HCID 111,2-DichloroethaneHCID 313Hydrochloric AcidHCID 6228DimethylformamideHCID 8471TriethylamineHCID 757711-HydroxybenzotriazoleHCID 1549481(2R)-2-(((tert-butoxy)carbonyl)amino)-3-(4-hydroxyphenyl)propanoic acidHCID 669880653-Butoxy-3-o-tolylazetidine trifluoroacetate

生成物 1

HCID 66988077[2-(3-butoxy-3-o-tolyl-azetidin-1-yl)-1-(4-hydroxybenzyl)-2-oxoethyl]-3-(3H-imidazol-4-yl)propionamide収率 90%

実験手順

205 mg (1.1 mmol) of EDC and then 145 mg (1.1 mmol) of HOBt are added to a solution of 250 mg (0.9 mmol) of (R)-2-tert-butoxycarbonylamino-3-(4-hydroxyphenyl)-propanoic acid in 5 ml of dimethylformamide. After stirring for 15 minutes at ambient temperature, 300 mg (1.1 mmol) of 3-butoxy-3-o-tolylazetidine trifluoro-acetate (described in Example 15.5) and 0.5 ml (3.6 mmol) of triethylamine are added. The reaction medium is stirred for 2 h at ambient temperature and then a 1N aqueous solution of hydrochloric acid is added and the mixture is extracted with ethyl acetate. The organic phase is washed with water, and then dried over magnesium sulphate, filtered and evaporated. The residue is purified by silica gel chromatography, elution being carried out with a 60/40 heptane/ethyl acetate mixture. 410 mg of [2-(3-butoxy-3-o-tolyl-azetidin-1-yl)-1-(4-hydroxybenzyl)-2-oxoethyl]-3-(3H-imidazol-4-yl)propionamide are obtained with a yield of 90%.

後処理

  1. stirringThe reaction medium is stirred for 2 h at ambient temperature
  2. extractionthe mixture is extracted with ethyl acetate
  3. washThe organic phase is washed with water
  4. dry with materialdried over magnesium sulphate
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue is purified by silica gel chromatography, elution

出典と根拠

ORDレコード
ord-7b3897ad785c40c2aa417f05a9557aaa
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08871187B2

反応ノート

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