Ethyl orthoformate → HCID 67517239、化合物

HRID 2173386ノート

反応式

HRID 2173386 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 67517239HCID 67517239、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8efdf79b83ab4d0eaed2e75c9aea0b78
出典データセット
uspto-grants-2015_06
特許番号
US09056859B2

反応ノート

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