Glycine → N-[(allyloxy)carbonyl]glycine

HRID 542362

反応式

HRID 542362 の反応式
[CH2:1]([O:4][C:5](Cl)=[O:6])[CH:2]=[CH2:3].[NH2:8][CH2:9][C:10]([OH:12])=[O:11]>O.[OH-].[Na+]>[CH2:1]([O:4][C:5]([NH:8][CH2:9][C:10]([OH:12])=[O:11])=[O:6])[CH:2]=[CH2:3]

参加物

5

反応物 2

HCID 750GlycineHCID 18052Allyl chloroformate

生成物 1

HCID 11964402N-[(allyloxy)carbonyl]glycine

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

12 ml of chloroformic acid allyl ester are added dropwise at 0° to a solution of 7.51 g of glycine in 20 ml of water and 44 ml of 5N NaOH solution. The suspension is then stirred for 16 hours at room temperature. After removal of the insoluble material by filtration, the filtrate is diluted with 100 ml of water and washed twice with CH2Cl2. The aqueous phase is adjusted to pH 2 with 4N HCl and extracted twice with CH2Cl2. The combined organic extracts are washed once with brine, dried over MgSO4 and concentrated by evaporation to form the white crystals of the title compound. IR in CH2Cl2 : 3450, 1715 cm-1.

後処理

  1. customAfter removal of the insoluble material
  2. filtrationby filtration
  3. additionthe filtrate is diluted with 100 ml of water
  4. washwashed twice with CH2Cl2
  5. extractionextracted twice with CH2Cl2
  6. washThe combined organic extracts are washed once with brine
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated by evaporation

出典と根拠

ORDレコード
ord-83912b56acc848b9ad4c34d49a828c72
出典データセット
uspto-grants-1987_04
特許番号
US04656165

関連ノート

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