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Diisopropylethylamine → HCID 18412024、化合物

HRID 992454
ノート
印刷プレビュー

反応式

HRID 992454 の反応式
Cl.[CH3:2][O:3][C:4]1[CH:5]=[C:6]([CH2:15][CH2:16][NH2:17])[CH:7]=[CH:8][C:9]=1[O:10][CH2:11][C:12]#[C:13]C.C(N(C(C)C)C(C)C)C.[Cl:27][C:28]1[CH:33]=[CH:32][C:31]([C:34]([OH:39])([CH3:38])[C:35](O)=[O:36])=[CH:30][CH:29]=1.F[P-](F)(F)(F)(F)F.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1>>[Cl:27][C:28]1[CH:29]=[CH:30][C:31]([C:34]([OH:39])([CH3:38])[C:35]([NH:17][CH2:16][CH2:15][C:6]2[CH:7]=[CH:8][C:9]([O:10][CH2:11][C:12]#[CH:13])=[C:4]([O:3][CH3:2])[CH:5]=2)=[O:36])=[CH:32][CH:33]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 81531DiisopropylethylamineHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 100130442-(4-Chlorophenyl)-2-hydroxypropanoic acidHCID 18412037HCID 18412037、化合物

生成物 1

HCID 18412024HCID 18412024、化合物

実験手順

To a stirred solution of 906 mg of 2-(3-methoxy-4-but-2-ynyloxy-phenyl)-ethylamine hydrochloride and 2.75 ml N-ethyldiisopropylamine are subsequently added 752 mg 2-(4-chlorophenyl)-2-hydroxy propionic acid and 1.875 g benzotriazole-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphate. The resulting clear solution is stirred over night, extracted with ethyl acetate. The extracts are washed several times with water, dried over sodium sulfate, filtered and evaporated. The resulting oily residue is purified on silicagel (hexanc ethyl acetate) to obtain the 2-(4-chlorophenyl)-2-hydroxy-N-[2-(3-methoxy-4-prop-2-ynyloxy-phenyl)-ethyl]propionamide.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe extracts are washed several times with water
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. customevaporated
  6. customThe resulting oily residue is purified on silicagel (hexanc ethyl acetate)

出典と根拠

ORDレコード
ord-33d0651326b04c7ebd7f11319889126b
出典データセット
uspto-grants-2002_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06469005B1

反応ノート

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