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Triethylamine → HCID 58869158、化合物

HRID 2355229
ノート
印刷プレビュー

反応式

HRID 2355229 の反応式
[C:1]1([S:7]([C:10]2[CH:19]=[C:18]3[C:13]([CH2:14][CH2:15][C@H:16]([CH2:20][NH:21][CH3:22])[O:17]3)=[CH:12][CH:11]=2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(N(CC)CC)C.BrC[C:32]([O:34][CH3:35])=[O:33]>CN1C(=O)CCC1>[CH3:35][O:34][C:32](=[O:33])[CH2:22][NH:21][CH2:20][C@H:16]1[CH2:15][CH2:14][C:13]2[C:18](=[CH:19][C:10]([S:7]([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)(=[O:9])=[O:8])=[CH:11][CH:12]=2)[O:17]1
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

5

反応物 3

HCID 8471TriethylamineHCID 60984Methyl bromoacetateHCID 58869134HCID 58869134、化合物

生成物 1

HCID 58869158HCID 58869158、化合物

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
0 °C

実験手順

(R)-(7-Benzenesulfonyl-chroman-2-ylmethyl)-methyl-amine (81 mg, 2.6 mmol) and triethylamine (0.2 mL) were added to 0.5 mL NMP and the mixture was cooled to 0° C. with stirring. Methyl 2-bromoacetate (26 uL) was added, and the reaction mixture was stirred for two hours at room temperature, then quenched by addition of water. The mixture was extracted with methylene chloride and the combined organic layers were washed with water and brine, dried (Na2SO4), filtered and contrated under reduced pressure. Purification of the residue by flash chromatography gave 40 mg of (R)-[(7-benzenesulfonyl-chroman-2-ylmethyl)-amino]-acetic acid methyl ester.

後処理

  1. stirringthe reaction mixture was stirred for two hours at room temperature
  2. customquenched by addition of water
  3. extractionThe mixture was extracted with methylene chloride
  4. washthe combined organic layers were washed with water and brine
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. customPurification of the residue by flash chromatography

出典と根拠

ORDレコード
ord-e3f5247f1f6949a79d4f50d3c6657c36
出典データセット
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07754759B2

反応ノート

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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