1,1'-Thiocarbonyldiimidazole → HCID 178506355, 화합물

HRID 1696679

반응식

HRID 1696679 반응식
[C:1](N1C=CN=C1)(N1C=CN=C1)=[S:2].[F:13][C:14]([F:25])([F:24])[O:15][C:16]1[CH:21]=[CH:20][C:19]([NH2:22])=[C:18]([NH2:23])[CH:17]=1>O1CCCC1>[SH:2][C:1]1[NH:23][C:18]2[CH:17]=[C:16]([O:15][C:14]([F:24])([F:25])[F:13])[CH:21]=[CH:20][C:19]=2[N:22]=1

참가 물질

4

반응물 2

HCID 802641,1'-ThiocarbonyldiimidazoleHCID 27739594-(Trifluoromethoxy)benzene-1,2-diamine

생성물 1

HCID 178506355HCID 178506355, 화합물수율 103.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

1,1′-thiocarbonyldiimidazole (1.13 g, 6.25 mmol) is added by portions to a solution of 4-(trifluoromethoxy)-ortho-phenylenediamine (1 g, 5.2 mmol) in 5 ml of tetrahydrofuran and the mixture is stirred at room temperature for 16 hours. The reaction mixture is then concentrated under reduced pressure and the residue is dissolved in 100 ml of ethyl acetate and washed with water (2×30 ml). The organic phase is then dried over MgSO4, filtered and concentrated. The residue is triturated in diisopropylether and pentane and dried under vacuum to yield 1.26 g of 2-mercapto-5-trifluoromethoxy-benzimidazole as a yellow powder. Quantitative yield. Analytical LC/MS (method B): retention time=3.69 min. m/z=235.67 (positive ion mode).

후처리

  1. concentrationThe reaction mixture is then concentrated under reduced pressure
  2. dissolutionthe residue is dissolved in 100 ml of ethyl acetate
  3. washwashed with water (2×30 ml)
  4. dry with materialThe organic phase is then dried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe residue is triturated in diisopropylether
  8. dry with materialpentane and dried under vacuum

출처 및 근거

ORD 기록
ord-b2377a823b6743a491300075ff1f4a6b
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08163768B2

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