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1-Butanol → 2-((2-(Trifluoromethyl)phenyl)formamido)acetic acid

HRID 64991
ノート
印刷プレビュー

反応式

HRID 64991 の反応式
[OH-:1].[Na+].[F:3][C:4]([F:15])([F:14])[C:5]1[CH:13]=[CH:12][CH:11]=[CH:10][C:6]=1[C:7](Cl)=[O:8].[CH2:16]([OH:20])[CH2:17]CC.[NH4+:21].[OH-]>NCC(O)=O.O.C(O)(C)C>[F:3][C:4]([F:15])([F:14])[C:5]1[CH:13]=[CH:12][CH:11]=[CH:10][C:6]=1[C:7]([NH:21][CH2:17][C:16]([OH:20])=[O:1])=[O:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 2631-ButanolHCID 14798Sodium HydroxideHCID 14923Ammonium HydroxideHCID 675612-(Trifluoromethyl)benzoyl chloride

生成物 1

HCID 167778182-((2-(Trifluoromethyl)phenyl)formamido)acetic acid

試薬・触媒・溶媒 3

HCID 750Glycine溶媒
HCID 962
Water
溶媒
2 回
HCID 3776Isopropanol溶媒

実験手順

In a 500 ml, 3-necked flask was dissolved glycine (9.03 g) in water (50 ml). The flask was cooled in an ice/methanol bath. Sodium hydroxide (12.6 g) in 30 cc of water was added. 2-Trifluoromethylbenzoyl chloride (25 g) was added at a temperature below 0° C. The bath was removed and the reaction mixture stirred for 2.5 hours at room temperature. To this was added concentrated HCl until the pH was 1. The solid was collected by filtration, washed with water and dried to give 25 g(84%), m.p. 147°-149° C. The product was a single spot by thin layer chromatography. (n-butyl alcohol:isopropyl alcohol:NH4OH; 10:4:4).

後処理

  1. temperatureThe flask was cooled in an ice/methanol bath
  2. customThe bath was removed
  3. additionTo this was added concentrated HCl until the pH was 1
  4. filtrationThe solid was collected by filtration
  5. washwashed with water
  6. customdried
  7. customto give 25 g(84%), m.p. 147°-149° C

出典と根拠

ORDレコード
ord-6c212c2210164fa8a5fe8c60c8c89f1c
出典データセット
uspto-grants-1986_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04612185

反応ノート

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