Hydrochloric Acid → HCID 86743789, 화합물

HRID 345359노트

반응식

HRID 345359 반응식
[CH2:1]([O:3][C:4]([N:6]1[CH2:10][CH2:9][C@@H:8]([CH2:11][CH:12]=O)[C@@H:7]1[C:14]([O:16][CH2:17][CH3:18])=[O:15])=[O:5])[CH3:2].[Cl-].[CH3:20][O:21]C[P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.CC(C)([O-])C.[K+].O1CCCC1.Cl>O1CCCC1>[CH2:1]([O:3][C:4]([N:6]1[CH2:10][CH2:9][C@@H:8]([CH2:11][CH2:12][CH:20]=[O:21])[C@@H:7]1[C:14]([O:16][CH2:17][CH3:18])=[O:15])=[O:5])[CH3:2]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 2723798Methoxymethyl-triphenylphosphonium chlorideHCID 66863523KOtBu THFHCID 86743787trans 1-Ethoxycarbonyl-2-ethoxycarbonylpyrrolidine-3-acetaldehyde

생성물 1

HCID 86743789HCID 86743789, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To 0.4 g of trans 1-ethoxycarbonyl-2-ethoxycarbonylpyrrolidine-3-acetaldehyde in 5 ml anhydrous tetrahydrofuran under nitrogen, cooled to -78°, is added dropwise a solution of 1.17 g of methoxymethyl-triphenylphosphonium chloride in 15 ml of anhydrous tetrahydrofuran to which is added 1.55 ml of potassium tert-butoxide/tetrahydrofuran (1.6M). Solution is stirred at room temperature for 4 hours. 2N Hydrochloric acid (11 ml) is added and the mixture is stirred for 45 minutes. The solution is concentrated and then extracted with methylene chloride. The extract is dried over sodium sulfate, filtered, concentrated, and the residue is purified by flash chromatography using ethyl acetate/hexane (1:5 to 3:7) to yield trans 1-ethoxycarbonyl-2-ethoxycarbonylpyrrolidine-3-propionaldehyde.

후처리

  1. stirringthe mixture is stirred for 45 minutes
  2. concentrationThe solution is concentrated
  3. extractionextracted with methylene chloride
  4. dry with materialThe extract is dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customthe residue is purified by flash chromatography

출처 및 근거

ORD 기록
ord-d5c2e7d8a4204c229a4f33c275520fec
출처 데이터셋
uspto-grants-1991_10
특허 번호
US05057506

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