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

HRID 502884
ノート
印刷プレビュー

反応式

HRID 502884 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 3939Lithium Hydroxide2 回HCID 574757172-Cyano-2-(2-nitro-5-phenoxy-benzyl)-hex-5-enoic acid ethyl ester2 回

生成物 1

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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒
HCID 962
Water
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1f4f3c287df741b2af5612b5da681308
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07776882B2

反応ノート

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