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Hydrochloric Acid → cis 4-Fluoromethyl-3-amino-2-oxo-azetidine hydrochloride

HRID 1199586
ノート
印刷プレビュー

反応式

HRID 1199586 の反応式
O.NN.[F:4][CH2:5][C@H:6]1[NH:9][C:8](=[O:10])[C@H:7]1[N:11]1C(=O)C2=CC=CC=C2C1=O.[ClH:22]>O1CCOCC1>[ClH:22].[F:4][CH2:5][C@H:6]1[NH:9][C:8](=[O:10])[C@H:7]1[NH2:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 24654Hydrazine hydrate (1:1)HCID 13244796cis 4-Fluoromethyl-3-phthalimido-2-oxo-azetidine

生成物 1

HCID 13244798cis 4-Fluoromethyl-3-amino-2-oxo-azetidine hydrochloride

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

14 ml of a solution of 1 ml of hydrazine hydrate in 50 ml of dioxane were added to a suspension of 1.24 g of the product of Step D in 1.2 ml of dioxane and the mixture was stirred at room temperature for 45 minutes and 5 ml of N hydrochloric acid were added thereto. The mixture was stirred for 15 hours and was evaporated to dryness. The residue was added to water and 2.3 ml of N hydrochloric acid with stirring and the mixture was filtered. Ethanol was added to the filtrate and the mixture was evaporated to dryness. Methanol was added to the residue followed by ethanol addition and the mixture was evaporated to dryness. The product was crystallized from methanol to obtain 0.391 g of cis 4-fluoromethyl-3-amino-2-oxo-azetidine hydrochloride melting at ≃220° C. (decomposition).

後処理

  1. stirringThe mixture was stirred for 15 hours
  2. customwas evaporated to dryness
  3. additionThe residue was added to water and 2.3 ml of N hydrochloric acid
  4. stirringwith stirring
  5. filtrationthe mixture was filtered
  6. additionEthanol was added to the filtrate
  7. customthe mixture was evaporated to dryness
  8. additionMethanol was added to the residue
  9. additionfollowed by ethanol addition
  10. customthe mixture was evaporated to dryness
  11. customThe product was crystallized from methanol

出典と根拠

ORDレコード
ord-dd284e3ef5814665860c3c0884b1f3c2
出典データセット
uspto-grants-1990_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04900728

反応ノート

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