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Dimethylformamide dimethyl acetal → HCID 69073013、化合物

HRID 733144
ノート
印刷プレビュー

反応式

HRID 733144 の反応式
[F:1][C:2]([F:19])([F:18])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([C:15](=[O:17])[CH3:16])[CH:10]=1.CO[CH:22](OC)[N:23]([CH3:25])[CH3:24]>CN(C=O)C>[CH3:22][N:23]([CH3:25])[CH:24]=[CH:16][C:15]([C:11]1[CH:10]=[C:9]([C:4]2[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=2[C:2]([F:18])([F:19])[F:1])[CH:14]=[CH:13][CH:12]=1)=[O:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 78373Dimethylformamide dimethyl acetalHCID 200997531-[2'-(Trifluoromethyl)[1,1'-biphenyl]-3-yl] ethanone

生成物 1

HCID 69073013HCID 69073013、化合物収率 95%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 1-(2′-trifluoromethyl-1,1′-biphenyl-3-yl)ethanone (0.325 g, 1.3 mmol) in DMF (1.45 mL) was added 1,1-dimethoxy-N,N-dimethylmethanamine (0.18 mL, 1.43 mL), and the solution was heated in a Smith Creator™ microwave reactor (commercially available from Personal Chemistry, Inc.) at 165° C. for 1200 seconds. The mixture was cooled to room temperature, partitioned between EtOAc and water, washed with brine, dried over sodium sulfate filtered and concentrated to give 0.395 g of the crude product (95%) (which was used as such for the subsequent step.

後処理

  1. temperaturethe solution was heated in a Smith Creator™ microwave reactor (commercially available from Personal Chemistry, Inc
  2. custompartitioned between EtOAc and water
  3. washwashed with brine
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-6bbd1ed0527b4bc4aaf817484cc2ff90
出典データセット
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07589116B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート