Hydrochloric Acid → 6-Bromo-5',6'-dihydro-4'H-spiro[chromene-2,3'-pyran]-4(3H)-imine

HRID 539355

반응식

HRID 539355 반응식
Cl.[Br:2][C:3]1[CH:4]=[C:5]2[C:15](=[CH:16][CH:17]=1)[O:14][C:8]1([CH2:13][CH2:12][CH2:11][O:10][CH2:9]1)[CH2:7][C:6]2=[N:18]S(C(C)(C)C)=O>O1CCOCC1>[Br:2][C:3]1[CH:4]=[C:5]2[C:15](=[CH:16][CH:17]=1)[O:14][C:8]1([CH2:13][CH2:12][CH2:11][O:10][CH2:9]1)[CH2:7][C:6]2=[NH:18]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 67979337N-(6-Bromo-5',6'-dihydro-4'H-spiro[chromene-2,3'-pyran]-4(3H)-ylidene)-2-methylpropane-2-sulfinamide

생성물 1

HCID 679793356-Bromo-5',6'-dihydro-4'H-spiro[chromene-2,3'-pyran]-4(3H)-imine

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

HCl (4 M in 1,4-dioxane) (0.395 mL, 12.99 mmol) was added to a suspension of N-(6-bromo-5′,6′-dihydro-4′H-spiro[chromene-2,3′-pyran]-4(3H)-ylidene)-2-methylpropane-2-sulfinamide (Example 45 Step 1, 520 mg, 1.30 mmol) in anhydrous 1,4-dioxane (6 mL) and the resulting mixture was stirred under a nitrogen atmosphere at r.t. for 2 days. A precipitate was formed. The precipitate was filtered off and washed with Et2O. The solid was then dissolved in DCM and sat. aq. NaHCO3. The mixture was poured into a phase separator, the organic layer was collected and concentrated. The title compound was used directly in the next step without any further purl fi cation.

후처리

  1. customA precipitate was formed
  2. filtrationThe precipitate was filtered off
  3. washwashed with Et2O
  4. dissolutionThe solid was then dissolved in DCM
  5. additionThe mixture was poured into a phase separator
  6. customthe organic layer was collected
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-749a79f4bf9c45f5a7b83968580c7727
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08865911B2

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