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Lithium hydroxide, monohydrate → HCID 22918353, 화합물

HRID 1376754
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HRID 1376754 반응식
C[O:2][C:3](=[O:28])[C:4]1[C:5](=[CH:10][C:11]([NH:21][C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)=[C:12]([NH:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH:13]=1)[C:6]([O:8]C)=[O:7].O.[OH-].[Li+]>CO.O>[NH:14]([C:12]1[CH:13]=[C:4]([C:3]([OH:28])=[O:2])[C:5](=[CH:10][C:11]=1[NH:21][C:22]1[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=1)[C:6]([OH:8])=[O:7])[C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1
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참가 물질

5

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 10407176dimethyl 4,5-dianilinobenzene-1,2-dicarboxylate

생성물 1

HCID 22918353HCID 22918353, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매2회

실험 절차

A steady stream of argon is passed through a suspension of 26.35 g (70.0 mmol) of 4,5-bis(anilino)phthalic acid dimethylester in 230 ml of methanol, and a solution of 11.78 g (280 mmol, 2 eq) of lithium hydroxide monohydrate in 116 ml of water is added. The reaction mixture is heated to reflux for 2.5 h, cooled to RT and diluted with 400 ml water. Methanol is removed by evaporation, the resulting solution is cooled to 0°, and 70 ml 4N hydrochloric acid are added. After 15 min. at 0°, the gray crystals are filtered off, washed with water and resuspended twice in 200 ml toluene with removal of the toluene by distillation to yield the title compound in the form of gray crystals, FAB-MS: 349 [M+ +H].

후처리

  1. temperatureThe reaction mixture is heated
  2. temperatureto reflux for 2.5 h
  3. customMethanol is removed by evaporation
  4. temperaturethe resulting solution is cooled to 0°
  5. addition70 ml 4N hydrochloric acid are added
  6. filtrationthe gray crystals are filtered off
  7. washwashed with water
  8. customresuspended twice in 200 ml toluene with removal of the toluene by distillation

출처 및 근거

ORD 기록
ord-a9e998fadeab4f659a0447833158b569
출처 데이터셋
uspto-grants-1997_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05663336

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