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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Hydrochloric Acid → cis 4-Fluoromethyl-3-amino-2-oxo-azetidine hydrochloride

HRID 345648
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HRID 345648 반응식
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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-610700972c4e43979364baa9b939ccae
출처 데이터셋
uspto-grants-1991_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05057512

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