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Benzoyl chloride → HCID 46673126、化合物

HRID 492985
ノート
印刷プレビュー

反応式

HRID 492985 の反応式
[CH2:1]([O:3][C:4]([CH2:6][N:7]1[CH2:12][CH2:11][NH:10][CH2:9][CH2:8]1)=[O:5])[CH3:2].C(N(CC)CC)C.[C:20](Cl)(=[O:27])[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1>O1CCCC1>[CH2:1]([O:3][C:4](=[O:5])[CH2:6][N:7]1[CH2:8][CH2:9][N:10]([C:20](=[O:27])[C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[CH2:11][CH2:12]1)[CH3:2]
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 3

HCID 7412Benzoyl chlorideHCID 8471TriethylamineHCID 207112Ethyl piperazine-1-acetate

生成物 1

HCID 46673126HCID 46673126、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

1-(Ethoxycarbonylmethyl)piperazine (5.1 g) was dissolved in tetrahydrofuran (300 ml) under a nitrogen atmosphere, and then triethylamine (8.25 ml) and benzoyl chloride (3.44 ml) were added thereto while cooling in an ice water bath, followed by warming to room temperature and stirring for 4 hrs. The reaction mixture was partitioned between ethyl acetate (200 ml) and a saturated aqueous solution of sodium hydrogencarbonate (100 ml). The organic layer was washed with a saturated aqueous solution of sodium hydrogencarbonate (100 ml), water (100 ml), brine (100 ml) and dried over anhydrous sodium sulfate. The solvent was evaporated to provide the titled compound (8.19 g, quant.) as a colorless oil.

後処理

  1. temperaturewhile cooling in an ice water bath
  2. customThe reaction mixture was partitioned between ethyl acetate (200 ml)
  3. washThe organic layer was washed with a saturated aqueous solution of sodium hydrogencarbonate (100 ml), water (100 ml), brine (100 ml)
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was evaporated

出典と根拠

ORDレコード
ord-b79b88e999514b578eba6a8200b055e2
出典データセット
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07531532B2

反応ノート

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