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

HRID 64991
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HRID 64991 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

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

생성물 1

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

시약·촉매·용매 3

HCID 750Glycine용매
HCID 962
Water
용매
2회
HCID 3776Isopropanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-6c212c2210164fa8a5fe8c60c8c89f1c
출처 데이터셋
uspto-grants-1986_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04612185

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