Hydrazine hydrate (1:1) → HCID 66768172, 화합물

HRID 2261677노트

반응식

HRID 2261677 반응식
[S:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[C:10](=[C:13]1[CH2:17][CH2:16][CH2:15][O:14]1)[C:11]#[N:12].O.[NH2:19][NH2:20]>C(O)C>[NH2:12][C:11]1[C:10]([C:2]2[S:1][C:5]3[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=3[N:3]=2)=[C:13]([CH2:17][CH2:16][CH2:15][OH:14])[NH:19][N:20]=1

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 66768211Benzothiazol-2-yl-(dihydrofuran-2-ylidene)-acetonitrile

생성물 1

HCID 66768172HCID 66768172, 화합물수율 67%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

The benzothiazol-2-yl-(dihydrofuran-2-ylidene)-acetonitrile (90 mg, 0.37 mmol) prepared above and hydrazine hydrate (25 mg, 0.5 mmol) were refluxed in ethanol (15 mL) for 10 hours. The solvent was evaporated and the resulting residue was triturated with dichloromethane. The solid was isolated by filtration and was then washed with dichloromethane and methanol to yield 60 mg (67%) of the title compound as a cream coloured solid. MS (m/z, ES+): 275.1 (M+1, 100). 1H NMR (300 MHz, ppm, DMSO-d6): δ (ppm), 11.5-12.2 (br s, 1H), 8.00 (d, 1H), 7.86 (d, 1H), 7.77 (t, 2H), 7.29 (t, 1H), 7.00-5.20 (br m, 2H), 4.55 (s, 1H), 3.52 (q, 2H), 2.83 (br s, 2H), 1.84 (q, 2H).

후처리

  1. customThe solvent was evaporated
  2. customthe resulting residue was triturated with dichloromethane
  3. customThe solid was isolated by filtration
  4. washwas then washed with dichloromethane and methanol

출처 및 근거

ORD 기록
ord-cb4141da96294b4f906819f00bf5f673
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07847101B2

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