Ethyl orthoformate → HCID 67517239, 화합물

HRID 2173386노트

반응식

HRID 2173386 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([OH:11])=[O:10])=[CH:4][C:3]=1[F:12].[CH:13](OCC)(OCC)OCC.[N-:23]=[N+:24]=[N-:25].[Na+]>CC(O)=O>[F:12][C:3]1[CH:4]=[C:5]([CH2:8][C:9]([OH:11])=[O:10])[CH:6]=[CH:7][C:2]=1[N:1]1[CH:13]=[N:25][N:24]=[N:23]1

참가 물질

5

반응물 3

HCID 31214Ethyl orthoformateHCID 33557Sodium AzideHCID 27783244-Amino-3-fluorophenylacetic acid

생성물 1

HCID 67517239HCID 67517239, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
100 °C

실험 절차

A solution of (4-amino-3-fluorophenyl)acetic acid (450 mg, 2.66 mmol) and triethyl orthoformate (1.18 g, 7.98 mmol) in HOAc (10 mL) was added sodium azide (208 mg, 3.19 mmol), and the mixture was heated to 100° C. for 3 hours. After the reaction was completed, the reaction mixture was cooled to ambient temperature. The solvent was removed under vacuum. The residue was dissolved in EtOAc, washed with water, dried over anhydrous sodium sulfate, and concentrated. The residue was directly used in next step.

후처리

  1. temperaturethe reaction mixture was cooled to ambient temperature
  2. customThe solvent was removed under vacuum
  3. dissolutionThe residue was dissolved in EtOAc
  4. washwashed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-8efdf79b83ab4d0eaed2e75c9aea0b78
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09056859B2

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