Triethylamine → HCID 68686408、化合物

HRID 1591697ノート

反応式

HRID 1591697 の反応式
Cl.[CH3:2][O:3][C:4](=[O:7])[CH2:5][NH2:6].CCN(CC)CC.[CH:15]1([CH2:18][O:19][C:20]2[CH:25]=[CH:24][C:23]([S:26](Cl)(=[O:28])=[O:27])=[CH:22][CH:21]=2)[CH2:17][CH2:16]1>O1CCOCC1.O>[CH3:2][O:3][C:4](=[O:7])[CH2:5][NH:6][S:26]([C:23]1[CH:22]=[CH:21][C:20]([O:19][CH2:18][CH:15]2[CH2:16][CH2:17]2)=[CH:25][CH:24]=1)(=[O:28])=[O:27]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 122755Glycine methyl ester hydrochlorideHCID 113686084-(cyclopropylmethoxy)benzenesulfonyl Chloride

生成物 1

HCID 68686408HCID 68686408、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒2 回

実験手順

To a solution of 7.125 g (56.75 mmol) of glycine methylester hydrochloride in 60 ml of dioxane and 24 ml of H2O, 15 ml (107.8 mmol) of Et3N and then a solution of 10 g (40.53 mmol) of 4-cyclopropylmethoxy-benzenesulfonyl chloride in 10 ml of dioxane are added dropwise at 0-5° C. After stirring for 3 h at r.t., the reaction is quenched with ice water and the mixture is extracted with AcOEt. The combined extracts are washed with H2O, brine, dried over MgSO4 and concentrated under reduced pressure to give the title compound as a colorless solid; 1H-NMR (400 MHz, CDCl3): 0.3-0.40 (m, 2H), 0.65-0.72 (m, 2H), 1.20-1.35 (m, 1H), 3.65 (m, 3H), 3.77 (d, 2H, J=5.04 Hz), 3.86 (d, 2H, J=7.08 Hz), 4.98 (brs, 1H), 6.96 (d, 2H, J=8.52 Hz), 7.77 (d, 2H, J=8.52 Hz).

後処理

  1. customthe reaction is quenched with ice water
  2. extractionthe mixture is extracted with AcOEt
  3. washThe combined extracts are washed with H2O, brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-89c9541a3b4d44818373a7ef7760953c
出典データセット
uspto-grants-2007_11
特許番号
US07291634B2

反応ノート

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