Ethyl 4-(1,4-dioxaspiro[4.5]dec-7-en-8-yl)benzoate → Ethyl 4-(1,4-dioxaspiro[4.5]dec-8-yl)benzoate

HRID 1255178

반응식

HRID 1255178 반응식
[O:1]1[C:5]2([CH2:10][CH2:9][C:8]([C:11]3[CH:21]=[CH:20][C:14]([C:15]([O:17][CH2:18][CH3:19])=[O:16])=[CH:13][CH:12]=3)=[CH:7][CH2:6]2)[O:4][CH2:3][CH2:2]1.[H][H]>CCOC(C)=O.[Pt](=O)=O>[O:1]1[C:5]2([CH2:10][CH2:9][CH:8]([C:11]3[CH:12]=[CH:13][C:14]([C:15]([O:17][CH2:18][CH3:19])=[O:16])=[CH:20][CH:21]=3)[CH2:7][CH2:6]2)[O:4][CH2:3][CH2:2]1

참가 물질

5

반응물 2

HCID 67159072Ethyl 4-(1,4-dioxaspiro[4.5]dec-7-en-8-yl)benzoateHCID 178418361HCID 178418361, 화합물2회

생성물 1

HCID 29921579Ethyl 4-(1,4-dioxaspiro[4.5]dec-8-yl)benzoate

시약·촉매·용매 2

HCID 345198Adams' catalyst촉매HCID 8857Ethyl Acetate용매

실험 절차

A solution of the title compound from Example 10 Step A (907 mg, 3.15 mmol) in EtOAc was degassed via nitrogen sparge. Platinum(IV) oxide (225 mgs, 0.991 mmol) was then added. The reaction flask was fitted with a 3-way adapter equipped with a hydrogen balloon. After 3 vacuum/hydrogen cycles, the reaction mixture was placed under a hydrogen atmosphere. After 1 h, the reaction mixture was filtered through a pad of Celite, rinsing with EtOAc, and concentrated in vacuo. The unpurified product was used in the subsequent step: LCMS m/z 291.0 [M+H]+.

후처리

  1. customsparge
  2. customThe reaction flask was fitted with a 3-way adapter
  3. filtrationthe reaction mixture was filtered through a pad of Celite
  4. washrinsing with EtOAc
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-22d40b0301c441768d0701ec469bca05
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08455638B2

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