tert-Butanol → HCID 67108500, 화합물

HRID 471882

반응식

HRID 471882 반응식
[CH2:1]([O:3][C:4]([C:6]1(CC=C)[CH2:11][CH2:10][CH2:9][CH:8]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH2:7]1)=[O:5])[CH3:2].C(=O)([O-])[O-:21].[K+].[K+].N12CCC(CC1)CC2.S([O-])([O-])=O.[Na+].[Na+].[C:40]([OH:44])(C)([CH3:42])[CH3:41]>O.[Fe-3](C#N)(C#N)(C#N)(C#N)(C#N)C#N.[K+].[K+].[K+]>[CH2:1]([O:3][C:4]([C:6]1([CH2:41][CH:40]([OH:44])[CH2:42][OH:21])[CH2:11][CH2:10][CH2:9][CH:8]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH2:7]1)=[O:5])[CH3:2]

참가 물질

8

반응물 5

HCID 6386tert-ButanolHCID 7527QuinuclidineHCID 11430Potassium CarbonateHCID 24437Sodium SulfiteHCID 67108610HCID 67108610, 화합물

생성물 1

HCID 67108500HCID 67108500, 화합물

시약·촉매·용매 2

HCID 178511488HCID 178511488, 화합물촉매HCID 962Water용매

실험 절차

To a solution of 1-allyl-cyclohexane-1,3-dicarboxylic acid diethyl ester from step 2 (250 g, 0.93 mol) in t-butanol (2.3 L) and water (2.3 L) was added potassium ferricyanide (920 g, 2.79 mol), potassium carbonate (386 g, 2.79 mol), potassium osmate dihydrate (4.75 g, 13 mmol) and quinuclidine (0.073 g, 7.0 mmol). The resulting dark colored solution was stirred at rt overnight and then quenched with portion-wise addition of sodium sulfite (1.05 kg, 8.37 mol). After dilution with ethyl acetate, it was extracted, washed with water and brine, dried over Na2SO4, and concentrated under reduced pressure. The resulting residue (224 g) was used in the next step without delay and without further purification.

후처리

  1. extractionAfter dilution with ethyl acetate, it was extracted
  2. washwashed with water and brine
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated under reduced pressure
  5. customThe resulting residue (224 g) was used in the next step without delay and without further purification

출처 및 근거

ORD 기록
ord-7468b90972ee44d690b9f8ca57c7a586
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08633190B2

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