Hydrazine hydrate (1:1) → HCID 66768172、化合物

HRID 407339ノート

反応式

HRID 407339 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 66768172HCID 66768172、化合物収率 67%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-0bd430dfa1904d3ab0e29348d80de771
出典データセット
uspto-grants-2014_06
特許番号
US08754233B2

反応ノート

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