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Hydrochloric Acid → HCID 53821538、化合物

HRID 1076308
ノート
印刷プレビュー

反応式

HRID 1076308 の反応式
[Cl:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=O)=[CH:4][CH:3]=1.[Cl:10][C:11]1[CH:32]=[CH:31][CH:30]=[CH:29][C:12]=1[CH2:13][C:14]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)([C:20](=[O:22])[CH3:21])[CH2:15][CH2:16][C:17]([OH:19])=[O:18].[OH-].[Na+].Cl>C(O)C.O>[Cl:10][C:11]1[CH:32]=[CH:31][CH:30]=[CH:29][C:12]=1[CH2:13][C:14]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)([C:20](=[O:22])[CH:21]=[CH:6][C:5]1[CH:8]=[CH:9][C:2]([Cl:1])=[CH:3][CH:4]=1)[CH2:15][CH2:16][C:17]([OH:19])=[O:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 77264-ChlorobenzaldehydeHCID 14798Sodium HydroxideHCID 103367854-(o-Chlorobenzyl)-4-phenyl-5-oxohexanoic acid

生成物 1

HCID 53821538HCID 53821538、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒
HCID 962
Water
溶媒

実験手順

p-Chlorobenzaldehyde (10.5 g., 0.075 mole) in ethanol (30 ml.) is added to a solution of levo-4-(2-chlorobenzyl)-4-phenyl-5-oxohexanoic acid (14.67 g., 0.045 mole) and sodium hydroxide (2.40 g., 0.06 mole) in water (150 ml.). The resulting mixture is heated on a steam bath for 24 hours. The reaction solution is cooled to room temperature, acidified with dilute hydrochloric acid (30 ml.), and the solid (yellow) which forms after scratching is filtered and air-dried to yield 24.1 g. of material with m.p. 150°-165°C. (sinters at 140°). Several recrystallizations from n-butyl chloride, followed by several recrystallizations from acetonitrile gives a white solid, m.p. 189°-190°C., [α]D25 = -61.5 (in 1% CHCl3).

後処理

  1. temperatureThe resulting mixture is heated on a steam bath for 24 hours
  2. filtrationthe solid (yellow) which forms after scratching is filtered
  3. customair-dried
  4. customto yield 24.1 g
  5. customwith m.p. 150°-165°C. (sinters at 140°)
  6. customSeveral recrystallizations from n-butyl chloride
  7. customfollowed by several recrystallizations from acetonitrile
  8. customgives a white solid, m.p. 189°-190°C., [α]D25 = -61.5 (in 1% CHCl3)

出典と根拠

ORDレコード
ord-f02eeda670b44987af5faf65219ff3ea
出典データセット
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03956374

反応ノート

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