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Toluene → 4-(4-(2-Amino-5-chloro-benzoyl)-phenoxymethyl) phenoxyacetic acid allyl ester

HRID 1975785
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HRID 1975785 반응식
[NH2:1][C:2]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][C:9]([OH:12])=[CH:8][CH:7]=1)=[O:5].C[Si]([N-][Si](C)(C)C)(C)C.[K+].C1(C)C=CC=CC=1.Br[CH2:36][C:37]1[CH:50]=[CH:49][C:40]([O:41][CH2:42][C:43]([O:45][CH2:46][CH:47]=[CH2:48])=[O:44])=[CH:39][CH:38]=1>CN(C=O)C>[CH2:46]([O:45][C:43](=[O:44])[CH2:42][O:41][C:40]1[CH:39]=[CH:38][C:37]([CH2:36][O:12][C:9]2[CH:8]=[CH:7][C:6]([C:4](=[O:5])[C:3]3[CH:13]=[C:14]([Cl:17])[CH:15]=[CH:16][C:2]=3[NH2:1])=[CH:11][CH:10]=2)=[CH:50][CH:49]=1)[CH:47]=[CH2:48]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 1140TolueneHCID 3251421Potassium bis(trimethylsilyl)amideHCID 10891412HCID 10891412, 화합물HCID 11402375Methanone, (2-amino-5-chlorophenyl)(4-hydroxyphenyl)-

생성물 1

HCID 545252454-(4-(2-Amino-5-chloro-benzoyl)-phenoxymethyl) phenoxyacetic acid allyl ester

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

A solution was formed by dissolving 2-amino-5-chloro-4'-hydroxybenzophenone (1.72 g, 8.07 mmol) in 40 mL of DMF. Potassium bis(trimethylsilyl)amide that was 0.5M in toluene (16.1 mL, 8.07 mmol, 1.0 equivalents) was added dropwise with stirring. Allyl 2-(4-bromomethylphenoxy)acetate (2.30 g, 8.07 mmol, 1.0 equivalents) was then added and the resulting orange slurry was stirred at ambient temperature for 45 minutes. The slurry was concentrated in vacuo, then diluted with CH2Cl2 (150 mL) and was extracted with 1N aqueous sodium bicarbonate (100 mL) and with 1N aqueous sodium chloride (100 mL), then dried over sodium sulfate and concentrated in vacuo to give the product as a yellow solid which was approximately 95% pure and was taken to the next step without purification. The product had Rf of 0.55 in 50:50:2 ethyl acetate/hexane/triethylamine. The structure was confirmed by proton NMR, carbon-13 NMR, and electron impact mass spectroscopy.

후처리

  1. customA solution was formed
  2. additionwas added dropwise
  3. stirringthe resulting orange slurry was stirred at ambient temperature for 45 minutes
  4. concentrationThe slurry was concentrated in vacuo
  5. additiondiluted with CH2Cl2 (150 mL)
  6. extractionwas extracted with 1N aqueous sodium bicarbonate (100 mL) and with 1N aqueous sodium chloride (100 mL)
  7. dry with materialdried over sodium sulfate
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-6b59b1aafdf74aed89cc771490f33e88
출처 데이터셋
uspto-grants-1994_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05288514

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