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Ammonia → HCID 21704275, 화합물

HRID 1106414
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HRID 1106414 반응식
[N+:1]([C:4]1[CH:9]=[C:8]([N+:10]([O-:12])=[O:11])[CH:7]=[CH:6][C:5]=1[NH:13][C:14]1[CH:22]=[CH:21][CH:20]=[CH:19][C:15]=1[C:16]([OH:18])=[O:17])([O-])=O.[Cl-].[NH4+].N.[S-2].[Na+].[Na+]>O.C(O)C>[NH2:1][C:4]1[CH:9]=[C:8]([N+:10]([O-:12])=[O:11])[CH:7]=[CH:6][C:5]=1[NH:13][C:14]1[CH:22]=[CH:21][CH:20]=[CH:19][C:15]=1[C:16]([OH:18])=[O:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 222AmmoniaHCID 14804Sodium SulfideHCID 25517Ammonium ChlorideHCID 6275142-(2,4-Dinitroanilino)benzoic acid

생성물 1

HCID 21704275HCID 21704275, 화합물수율 67.1%

시약·촉매·용매 2

HCID 702Ethanol용매
HCID 962
Water
용매

실험 절차

1.80 g (6 mmol) of 2-(2,4-dinitrophenylamino) benzoic acid, 2.66 g (42.6 mmol) of ammonium chloride, 2.4 ml of ammonia, concentrated, 52 ml of ethanol, and 21 ml of distilled water are combined at an internal temperature of 78° C. (bath temperature 90° C.). To this batch is added, in 3 portions, 4.44 g (20 mmol) of sodium sulfide (35% strength) and the mixture is stirred for one hour. The batch is suctioned off at room temperature and washed in succession with water and ether. The filtrate is concentrated to the aqueous phase and extracted by shaking with ethyl acetate. The organic phase is dried, filtered, and concentrated. The aqueous phase is acidified with 1N hydrochloric acid and suctioned off, thus obtaining 1.1 g of 2-(2-amino-4-nitrophenylamino)benzoic acid (processed without purification).

후처리

  1. customare combined at an internal temperature of 78° C. (bath temperature 90° C.)
  2. customis suctioned off at room temperature
  3. washwashed in succession with water and ether
  4. concentrationThe filtrate is concentrated to the aqueous phase
  5. extractionextracted
  6. stirringby shaking with ethyl acetate
  7. customThe organic phase is dried
  8. filtrationfiltered
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-c35494331f674ded8d50704645d93ab7
출처 데이터셋
uspto-grants-2000_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06057304

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