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Hydrochloric Acid → 2-Cyano-2-(2-nitro-5-phenoxy-benzyl)-hex-5-enoic acid

HRID 502884
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HRID 502884 반응식
C([O:3][C:4](=[O:29])[C:5]([C:27]#[N:28])([CH2:10][C:11]1[CH:16]=[C:15]([O:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH:14]=[CH:13][C:12]=1[N+:24]([O-:26])=[O:25])[CH2:6][CH2:7][CH:8]=[CH2:9])C.[Li+].[OH-].Cl>CO.O>[C:27]([C:5]([CH2:10][C:11]1[CH:16]=[C:15]([O:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH:14]=[CH:13][C:12]=1[N+:24]([O-:26])=[O:25])([CH2:6][CH2:7][CH:8]=[CH2:9])[C:4]([OH:29])=[O:3])#[N:28]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 3939Lithium Hydroxide2회HCID 574757172-Cyano-2-(2-nitro-5-phenoxy-benzyl)-hex-5-enoic acid ethyl ester2회

생성물 1

HCID 574757182-Cyano-2-(2-nitro-5-phenoxy-benzyl)-hex-5-enoic acid

시약·촉매·용매 2

HCID 887Methanol용매
HCID 962
Water
용매

실험 절차

2-cyano-2-(2-nitro-5-phenoxy-benzyl)-hex-5-enoic acid ethyl ester (2.84 g, 7.20 mmol) was dissolved in methanol (42 mL). In a separate flask LiOH (1.5 g, 36.0 mmol) was dissolved in water (21 mL). The LiOH solution was added to the methanolic solution containing 2-cyano-2-(2-nitro-5-phenoxy-benzyl)-hex-5-enoic acid ethyl ester and the reaction was allowed to stir at room temperature for 2 hours. Next, 12N HCl (3 mL) was added to the reaction mixture followed by removal of the methanol under reduced pressure. The reaction mixture was poured into a separatory funnel, ethyl acetate was added and the organic layer washed 2 times with 1N HCl and one time with saturated brine solution. The organic layer was separated, dried with sodium sulfate, filtered and the solvent was removed to yield a residue.

후처리

  1. customfollowed by removal of the methanol under reduced pressure
  2. additionThe reaction mixture was poured into a separatory funnel
  3. additionethyl acetate was added
  4. washthe organic layer washed 2 times with 1N HCl and one time with saturated brine solution
  5. customThe organic layer was separated
  6. dry with materialdried with sodium sulfate
  7. filtrationfiltered
  8. customthe solvent was removed
  9. customto yield a residue

출처 및 근거

ORD 기록
ord-1f4f3c287df741b2af5612b5da681308
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07776882B2

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