Sodium Carbonate → 2-Sulfanilamido-1,3,4-thiadiazole

HRID 1854259ノート

反応式

HRID 1854259 の反応式
[S:1]1[CH:5]=[N:4][N:3]=[C:2]1[NH:6][S:7]([C:10]1[CH:15]=[CH:14][C:13]([NH:16]C(=O)C)=[CH:12][CH:11]=1)(=[O:9])=[O:8].C([O-])([O-])=O.[Na+].[Na+]>Cl>[NH2:16][C:13]1[CH:14]=[CH:15][C:10]([S:7]([NH:6][C:2]2[S:1][CH:5]=[N:4][N:3]=2)(=[O:9])=[O:8])=[CH:11][CH:12]=1

参加物

4

反応物 2

HCID 10340Sodium CarbonateHCID 694845N-(4-(N-1,3,4-thiadiazol-2-ylsulfamoyl)phenyl)acetamide

生成物 1

HCID 2347622-Sulfanilamido-1,3,4-thiadiazole収率 50%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

Compound 102 (1.0 g, 3.6 mmol) was suspended in 3N HCl (10 mL) and heated to reflux for 30 min. The acidic mixture was neutralized with Na2CO3 solution. The precipitated product was collected by filtration, washed with water, and dried to give the product (450 mg, 1.8 mmol, 49%), mp 226° C. (lit2 mp 221-222° C.); 1H NMR (250 MHz, CDCl3) δ 5.95 (2, s), 6.57 (2, d, J=6.5 Hz), 7.41 (2, d, J=6.5 Hz), 8.68 (1, s), 14.03 (1, br s).

後処理

  1. temperatureheated
  2. temperatureto reflux for 30 min
  3. filtrationThe precipitated product was collected by filtration
  4. washwashed with water
  5. customdried

出典と根拠

ORDレコード
ord-e4a9b8136d1e4709b9384953406c9516
出典データセット
uspto-grants-2015_02
特許番号
US08962663B2

反応ノート

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