Formaldehyde → HCID 66636594、化合物

HRID 44250ノート

反応式

HRID 44250 の反応式
[NH:1]1[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.[NH:7]1[CH:11]=[CH:10][CH:9]=[CH:8]1.[CH2:12]=O.[OH-].[Na+]>C(O)(=O)C>[NH:7]1[CH:11]=[CH:10][CH:9]=[C:8]1[CH2:12][N:1]1[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1

参加物

6

反応物 4

HCID 712FormaldehydeHCID 8027PyrroleHCID 8083MorpholineHCID 14798Sodium Hydroxide

生成物 1

HCID 66636594HCID 66636594、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To a solution of morpholine (22 mmoles) in acetic acid (10 ml) there is added pyrrole (20 mmoles) dropwise at 0° C. Formaldehyde (37% aq., 20 mmoles) is then added dropwise. The reaction mixture is stirred for 2 hours at ambient temperature. The solution is cooled to 0° C. and is brought to alkaline pH (10-11) using 20% aqueous NaOH solution. After extraction with DCM, the organic phases are washed with water and with saturated aqueous NaCl solution, dried over sodium sulphate, filtered and evaporated to dryness to yield the title product in the form of a white solid which is used directly in the next Step.

後処理

  1. temperatureThe solution is cooled to 0° C.
  2. extractionAfter extraction with DCM
  3. washthe organic phases are washed with water and with saturated aqueous NaCl solution
  4. dry with materialdried over sodium sulphate
  5. filtrationfiltered
  6. customevaporated to dryness

出典と根拠

ORDレコード
ord-ac96ec0ecba344c39e16f6c953d0cc35
出典データセット
uspto-grants-2013_09
特許番号
US08541412B2

反応ノート

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