Sulfuric Acid → HCID 178433434、化合物

HRID 1926226ノート

反応式

HRID 1926226 の反応式
S(=O)(=O)(O)O.CO[CH:8](OC)[C:9]([NH:11][CH:12]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[CH3:13])=[O:10]>>[CH3:13][C:12]1[C:14]2[C:19](=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH:8]=[C:9]([OH:10])[N:11]=1

参加物

3

反応物 2

HCID 1118Sulfuric AcidHCID 214193672,2-Dimethoxy-N-(1-phenylethyl)acetamide

生成物 1

HCID 178433434HCID 178433434、化合物

反応条件

温度
60 °C

実験手順

Concentrated sulfuric acid (18 M; 6.0 mL) was added to 2,2-dimethoxy-N-(1-phenylethyl)-acetamide (2.49 g, 11.2 mmol), and the resulting solution was stirred at 60° C. for 105 min. The reaction mixture was added to ≈100 mL of ice, and the yellow precipitate was filtered off. The pH of the filtrate was adjusted to 7-8 with NaHCO3 solution, the initial yellow solid was added, and the yellow precipitate was filtered off, washed with water, and dried in vacuo, giving the title compound as yellow solid. 1H NMR (400 MHz, DMSO-d6): δ=10.68 (brs, 1H), 8.00 (dd, J=1.0, 8.6 Hz, 1H), 7.64 (d, J=8.4 Hz, 1H), 7.53 (dt, J=1.0, 8.0 Hz, 1H), 7.28 (dt, J=0.8, 8.0 Hz, 1H), 6.69 (s, 1H), 2.78 (s, 3H). MS(ES+): m/z=160.10 (100) [MH+]. HPLC: tR=2.13 min (polar—5 min, ZQ3).

後処理

  1. filtrationthe yellow precipitate was filtered off
  2. additionthe initial yellow solid was added
  3. filtrationthe yellow precipitate was filtered off
  4. washwashed with water
  5. customdried in vacuo

出典と根拠

ORDレコード
ord-6ec65041e275411a864579f35a0372ae
出典データセット
uspto-grants-2012_05
特許番号
US08178668B2

反応ノート

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