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O-Phenylenediamine → HCID 22139864, 화합물

HRID 1825917
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인쇄 미리보기

반응식

HRID 1825917 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH2:8].[Cl:9][C:10]1[C:11]([N:15]=[C:16]=[S:17])=[CH:12][S:13][CH:14]=1>C1COCC1>[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH:8][C:16]([NH:15][C:11]1[C:10]([Cl:9])=[CH:14][S:13][CH:12]=1)=[S:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 7243O-PhenylenediamineHCID 22139828HCID 22139828, 화합물

생성물 1

HCID 22139864HCID 22139864, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

0.86 g of 1,2-diaminobenzene (o-phenylenediamine) is added to a solution of 1.4 g of 4-chloro-3-thienyl isothiocyanate in 40 ml of anhydrous THF, the mixture is stirred at room temperature for about 20 hours and the solvent is distilled off under reduced pressure. The residue is treated with water and extracted with ethyl acetate, the solvent is distilled off again and the residue is purified using medium-pressure silica gel column chromatography using a 1:1 mixture of ethyl acetate and toluene. Brown-yellow solid.

후처리

  1. distillationthe solvent is distilled off under reduced pressure
  2. additionThe residue is treated with water
  3. extractionextracted with ethyl acetate
  4. distillationthe solvent is distilled off again
  5. customthe residue is purified
  6. additiona 1:1 mixture of ethyl acetate and toluene

출처 및 근거

ORD 기록
ord-c76248537d2e4cf2aad7baaa95255734
출처 데이터셋
uspto-grants-2006_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07049333B2

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