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Water → HCID 54424346, 화합물

HRID 1275958
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HRID 1275958 반응식
[C:1]([O:4][C:5](=O)[CH3:6])(=[O:3])[CH3:2].[CH3:8][C:9]1([CH3:21])[C:13]([CH3:14])=[CH:12][CH2:11][CH:10]1[CH:15]=[CH:16][CH2:17]C(O)C.O>CN(C)C1C=CN=CC=1.CC(OC)(C)C>[CH3:8][C:9]1([CH3:21])[C:13]([CH3:14])=[CH:12][CH2:11][CH:10]1[CH:15]=[CH:16][CH2:17][CH:5]([O:4][C:1](=[O:3])[CH3:2])[CH3:6]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 962WaterHCID 7918Acetic AnhydrideHCID 1068064-Penten-2-ol, 5-(2,2,3-trimethyl-3-cyclopenten-1-yl)-

생성물 1

HCID 54424346HCID 54424346, 화합물수율 95%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 15413tert-Butyl methyl ether
용매

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온도
52.5 °C

실험 절차

50 g (0.48 mol) of acetic anhydride was added dropwise to the solution of 78.6 g (0.40 mol) of 5-(2,2,3-trimethylcyclopent-3-enyl)pent-4-en-2-ol and 5.0 g of 4-dimethylaminopyridine in 150 ml of MTBE. The reaction mixture was stirred at 50-55° C. for 1 hour, treated with 0.5 l of water and extracted with 3×150 ml of hexane. The combined organic layers were neutralized with aqueous potassium hydrogen carbonate solution, washed with water, dried (MgSO4) and evaporated in vacuo. The residue (102 g) was distilled at 80-81° C./0.2 Torr to give 89.8 g (95% yield) of acetic acid 5-(2,2,3-trimethyl-cyclopent-3-enyl)pent-4-en-2-yl ester.

후처리

  1. extractionextracted with 3×150 ml of hexane
  2. washwashed with water
  3. dry with materialdried (MgSO4)
  4. customevaporated in vacuo
  5. distillationThe residue (102 g) was distilled at 80-81° C./0.2 Torr

출처 및 근거

ORD 기록
ord-fbb6b26b32e7453b976a3feb223574f0
출처 데이터셋
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06162954

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