Hydrochloric Acid → HCID 15267964, 화합물

HRID 523324

반응식

HRID 523324 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 15267964HCID 15267964, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-13e301d3f8b6427b8583f3952c60cbcd
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09334366B2

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