Morpholine → Ethyl 2-methyl-4-morpholinobutyrate

HRID 267352

反応式

HRID 267352 の反応式
Br[CH2:2][CH2:3][CH:4]([CH3:10])[C:5]([O:7][CH2:8][CH3:9])=[O:6].[NH:11]1[CH2:16][CH2:15][O:14][CH2:13][CH2:12]1>C1C=CC=CC=1>[CH3:10][CH:4]([CH2:3][CH2:2][N:11]1[CH2:16][CH2:15][O:14][CH2:13][CH2:12]1)[C:5]([O:7][CH2:8][CH3:9])=[O:6]

参加物

4

反応物 2

HCID 8083MorpholineHCID 12780980Ethyl 4-bromo-2-methylbutanoate

生成物 1

HCID 21418135Ethyl 2-methyl-4-morpholinobutyrate

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A mixture of 40.0 g. (0.19 mole) of ethyl 4-bromo-2-methylbutyrate (Tetrahedron 21, 2966 (1965)), 66.0 g. (0.76 mole) of morpholine and 750 ml. of benzene was heated at 60°C. for 5 hours and stirred at room temperature for a total of 40 hours. A colorless solid was removed by filtration, and the mother liquor was evaporated to give a colorless, mobile residue. This material was combined with 250 ml. of ether and filtered to remove a small amount of additional solid. The solution was concentrated and the residue distilled to give the desired material as 38.0 g. (93%) of colorless liquid (b.p. 71°-73°C. at 0.10 mm).

後処理

  1. additionA mixture of 40.0 g
  2. customA colorless solid was removed by filtration
  3. customthe mother liquor was evaporated
  4. customto give a colorless, mobile residue
  5. filtrationof ether and filtered
  6. customto remove a small amount of additional solid
  7. concentrationThe solution was concentrated
  8. distillationthe residue distilled

出典と根拠

ORDレコード
ord-3b6645cb1cf4455798acf0fc34c234e3
出典データセット
uspto-grants-1976_03
特許番号
US03941782

関連ノート

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