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Sodium Bicarbonate → HCID 178449933, 화합물

HRID 1906696
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HRID 1906696 반응식
[C:1]([CH:6]1[C:11](=[O:12])[CH2:10][CH:9]([CH:13]2[CH2:19][CH2:18][O:17][CH:16]([CH:20]([CH3:22])[CH3:21])[O:15][CH2:14]2)[CH2:8][C:7]1=[O:23])(=O)[CH2:2][CH2:3][CH3:4].[Cl-].[CH2:25]([O:27][NH3+:28])[CH3:26].C(=O)(O)[O-].[Na+]>CO>[CH2:25]([O:27][NH:28][C:1](=[C:6]1[C:11](=[O:12])[CH2:10][CH:9]([CH:13]2[CH2:19][CH2:18][O:17][CH:16]([CH:20]([CH3:22])[CH3:21])[O:15][CH2:14]2)[CH2:8][C:7]1=[O:23])[CH2:2][CH2:3][CH3:4])[CH3:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 13473084HCID 13473084, 화합물HCID 19001768HCID 19001768, 화합물

생성물 1

HCID 178449933HCID 178449933, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

6.5 parts by weight of 2-butyryl-5-(2-isopropyl-1,3-dioxepan-5-yl)-cyclohexane-1,3-dione, 2.1 parts by weight of ethoxyammonium chloride and 1.8 parts by weight of sodium bicarbonate in 80 parts by volume of methanol are stirred for 16 hours at room temperature. The solvent is distilled off under reduced pressure, the residue is stirred with 50 parts by volume of water and 50 parts by volume of dichloromethane, the organic phase is separated off, the aqueous phase is extracted once with 50 parts by volume of dichloromethane, the combined organic phases are dried over sodium sulfate, and the solvent is distilled off under reduced pressure. 6.2 parts by weight of 2-(1-ethoxyamino-n-butylidene)-5-(2-isopropyl1,3-dioxepan-5-yl)-cyclohexane-1,3-dione are obtained as an oil (active ingredient No. 1).

후처리

  1. distillationThe solvent is distilled off under reduced pressure
  2. customthe organic phase is separated off
  3. extractionthe aqueous phase is extracted once with 50 parts by volume of dichloromethane
  4. dry with materialthe combined organic phases are dried over sodium sulfate
  5. distillationthe solvent is distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-efad078866f64c24ab5a3d1d248f69ab
출처 데이터셋
uspto-grants-1987_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04654073

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