Morpholine → Morpholine, 4-(isocyanoacetyl)-

HRID 1423869ノート

反応式

HRID 1423869 の反応式
[N+:1]([CH2:3][C:4](OC)=[O:5])#[C-:2].[NH:8]1[CH2:13][CH2:12][O:11][CH2:10][CH2:9]1>>[N+:1]([CH2:3][C:4]([N:8]1[CH2:13][CH2:12][O:11][CH2:10][CH2:9]1)=[O:5])#[C-:2]

参加物

3

反応物 2

HCID 8083MorpholineHCID 547815Methyl isocyanoacetate

生成物 1

HCID 6455475Morpholine, 4-(isocyanoacetyl)-収率 58%

実験手順

Prepared in accordance with Method B with methyl isocyanoacetate (2.51 g, 25.30 mmol) and morpholine (3.30 mL, 38.05 mmol). The reaction mixture was stirred 24 h at RT and then concentrated. The residue was dissolved in dichloromethane (50 mL) and the organic layer was washed with 10% aqueous citric acid (2×25 mL), dried over MgSO4, filtered and evaporated. 2-Isocyano-1-morpholinoethanone SLA 07118 was obtained as a brown oil (2.28 g, 58% yield).

後処理

  1. concentrationconcentrated
  2. dissolutionThe residue was dissolved in dichloromethane (50 mL)
  3. washthe organic layer was washed with 10% aqueous citric acid (2×25 mL)
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customevaporated

出典と根拠

ORDレコード
ord-303b536dbf55423fb1168644c2f6e458
出典データセット
uspto-grants-2015_01
特許番号
US08927589B2

反応ノート

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