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Hydrochloric Acid → HCID 67499245, 화합물

HRID 661353
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HRID 661353 반응식
[Cl:1][C:2]1[C:3]([C:8]2([F:18])[CH2:17][CH2:16][C:11]3(OCC[O:12]3)[CH2:10][CH2:9]2)=[N:4][CH:5]=[CH:6][CH:7]=1.Cl>O1CCOCC1>[Cl:1][C:2]1[C:3]([C:8]2([F:18])[CH2:9][CH2:10][C:11](=[O:12])[CH2:16][CH2:17]2)=[N:4][CH:5]=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 67499172HCID 67499172, 화합물

생성물 1

HCID 67499245HCID 67499245, 화합물수율 103.4%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

To a solution of the product of Example 1B (3.0 g, 11.04 mmol) in dioxane (50 mL) was added 3M HCl (50 mL). The reaction mixture was stirred overnight at ambient temperature, quenched with 3M NaOH (50 mL) and extracted with ethyl acetate. The organic layer was separated and concentrated. The resulting residue was chromatographed on silica gel eluting with 0%-30% ethyl acetate-hexane to obtain 95% pure desired product (2.6 g, 103%) as a white solid. 1H NMR (300 MHz, DMSO-d6) δ PPM 2.29-2.37 (M, 2H), 2.54-2.75 (M, 6H), 7.48 (DDD, J=8.14, 4.75, 1.02 HZ, 1H), 8.01 (DD, J=8.14, 1.70 HZ, 1H), 8.54 (D, J=4.75 HZ, 1H). MS (DCI) M/Z 228.01 (M+H)+.

후처리

  1. customquenched with 3M NaOH (50 mL)
  2. extractionextracted with ethyl acetate
  3. customThe organic layer was separated
  4. concentrationconcentrated
  5. customThe resulting residue was chromatographed on silica gel eluting with 0%-30% ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-1e3d7996fe014e7da85f36d46903fdfc
출처 데이터셋
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08084616B2

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