Acetic Acid → HCID 86594213, 화합물

HRID 456364

반응식

HRID 456364 반응식
[NH2:1][C:2]1[CH:3]=[C:4]([C:9]2[CH:15]=[CH:14][C:12]([NH2:13])=[C:11]([NH2:16])[CH:10]=2)[CH:5]=[CH:6][C:7]=1[NH2:8].C(O)(=O)C>CC(C)=O>[C:2](=[NH:1])([CH3:3])[CH3:7].[NH2:1][C:2]1[CH:3]=[C:4]([C:9]2[CH:15]=[CH:14][C:12]([NH2:13])=[C:11]([NH2:16])[CH:10]=2)[CH:5]=[CH:6][C:7]=1[NH2:8].[C:2](=[NH:1])([CH3:3])[CH3:7].[C:2](=[NH:1])([CH3:3])[CH3:7].[NH2:1][C:2]1[CH:3]=[C:4]([C:9]2[CH:15]=[CH:14][C:12]([NH2:13])=[C:11]([NH2:16])[CH:10]=2)[CH:5]=[CH:6][C:7]=1[NH2:8]

참가 물질

5

반응물 2

HCID 176Acetic AcidHCID 70713,3'-Diaminobenzidine

생성물 2

HCID 86594213HCID 86594213, 화합물HCID 86594214HCID 86594214, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

In a 200-ml flask equipped with a Soxhlet extractor including molecular sieves 4A as a dehydrating agent, a stirrer, a condenser and a thermometer were placed 21.4 g (100 mmol) of 3,3′-diaminobenzidine, 100 ml of acetone and 3.0 g (50 mmol) of acetic acid, followed by heating under reflux in a nitrogen atmosphere for 3 hours. After cooling to room temperature, acetone was removed under reduced pressure, and the residue was purified by silica gel chromatography to yield 16.5 g (65 mmol) of 3,3′-diaminobenzidine monoisopropanimine [N′-isopropylidene-3,4,3′,4′-biphenyltetramine] and 4.7 g (16 mmol) of 3,3′-diaminobenzidine diisopropanimine [N′,N′″-diisopropylidene-3,4,3′,4′-biphenyltetramine].

후처리

  1. customIn a 200-ml flask equipped with a Soxhlet extractor
  2. temperatureby heating
  3. temperatureunder reflux in a nitrogen atmosphere for 3 hours
  4. customacetone was removed under reduced pressure
  5. customthe residue was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-1d55ecfb0ec9447baf09db486c82d860
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07186454B2

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