Hydrochloric Acid → HCID 15267964、化合物

HRID 523324

反応式

HRID 523324 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([C:22](O)=[O:23])[C:7]([C:10]2[C:11]([C:19](O)=[O:20])=[CH:12][C:13]([N+:16]([O-:18])=[O:17])=[CH:14][CH:15]=2)=[CH:8][CH:9]=1)([O-:3])=[O:2].O.Cl>C1COCC1>[N+:1]([C:4]1[CH:5]=[C:6]([CH2:22][OH:23])[C:7]([C:10]2[C:11]([CH2:19][OH:20])=[CH:12][C:13]([N+:16]([O-:18])=[O:17])=[CH:14][CH:15]=2)=[CH:8][CH:9]=1)([O-:3])=[O:2]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 962WaterHCID 97509(1,1'-Biphenyl)-2,2'-dicarboxylic acid, 4,4'-dinitro-

生成物 1

HCID 15267964HCID 15267964、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

80 g (241 mmol) 4,4′-Dinitro-1,1′-biphenyl-2,2′-dicarboxylic acid are dissolved in 225 ml THF and added dropwise in the course of 1 hour to 1.4 L (1440 mmol) of a borane-tetrahydrofuran complex 1.0 M solution in THF. After 19 hours at 25° C., 500 ml of water are carefully added. After 1 hour, the solution is acidified to pH=1-2 with 30 ml of 1N HCl solution and allowed to stirred for 30 min. The reaction mixture is then partitioned between ethyl acetate and water. The organic phase is washed repeatedly with water, dried over sodium sulfate, filtered and concentrated by rotary evaporation. The residue, 48 g (66%) of 2,2′-bis(hydroxymethyl)-4,4′-dinitro-1,1′-biphenyl as white powder is used without further purification.

後処理

  1. waitAfter 1 hour
  2. customThe reaction mixture is then partitioned between ethyl acetate and water
  3. washThe organic phase is washed repeatedly with water
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated by rotary evaporation
  7. customThe residue, 48 g (66%) of 2,2′-bis(hydroxymethyl)-4,4′-dinitro-1,1′-biphenyl as white powder is used without further purification

出典と根拠

ORDレコード
ord-13e301d3f8b6427b8583f3952c60cbcd
出典データセット
uspto-grants-2016_05
特許番号
US09334366B2

関連ノート

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