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Hydrochloric Acid → 1-(2-Hydroxyethyl)piperazin-2-one

HRID 639991
ノート
印刷プレビュー

反応式

HRID 639991 の反応式
[Si]([O:8][CH2:9][CH2:10][N:11]1[CH2:16][CH2:15][N:14](C(OC(C)(C)C)=O)[CH2:13][C:12]1=[O:24])(C(C)(C)C)(C)C.Cl>O1CCOCC1>[OH:8][CH2:9][CH2:10][N:11]1[CH2:16][CH2:15][NH:14][CH2:13][C:12]1=[O:24]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 68638537Tert-butyl 4-(2-{[tert-butyl(dimethyl)silyl]oxy}ethyl)-3-oxopiperazine-1-carboxylate

生成物 1

HCID 132438661-(2-Hydroxyethyl)piperazin-2-one収率 57%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

A mixture of tert-butyl 4-(2-{[tert-butyl(dimethyl)silyl]oxy}ethyl)-3-oxopiperazine-1-carboxylate (3.4 g, 9.50 mmol) and hydrogen chloride (15 ml of a 4M solution in 1,4-dioxane) in 1,4-dioxane (10 ml) was stirred at room temperature for 4 hour and then the mixture was evaporated. The residue was dissolved in a mixture of 5% methanol in dichloromethane (30 ml), basified with a 7N solution of ammonia in methanol and then filtered. The filtrate was evaporated and the residue was purified by silica gel chromatography eluting with 10% methanol in dichloromethane containing 0-5% 7M ammonia in methanol to give 1-(2-hydroxyethyl)piperazin-2-one (0.708 g, 57% yield) as a pale yellow oil.

後処理

  1. customthe mixture was evaporated
  2. dissolutionThe residue was dissolved in a mixture of 5% methanol in dichloromethane (30 ml)
  3. filtrationfiltered
  4. customThe filtrate was evaporated
  5. customthe residue was purified by silica gel chromatography
  6. washeluting with 10% methanol in dichloromethane containing 0-5% 7M ammonia in methanol

出典と根拠

ORDレコード
ord-87449b1ef112498dad7f80abeec664e3
出典データセット
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07691867B2

反応ノート

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