Hydrochloric Acid → HCID 49780164、化合物

HRID 929505ノート

反応式

HRID 929505 の反応式
[F:1][C:2]([F:28])([F:27])[O:3][C:4]1[CH:9]=[CH:8][C:7]([NH:10][C:11](=[O:26])[NH:12][CH:13]2[CH2:18][CH2:17][N:16](C(OC(C)(C)C)=O)[CH2:15][CH2:14]2)=[CH:6][CH:5]=1.Cl>CO>[NH:16]1[CH2:17][CH2:18][CH:13]([NH:12][C:11]([NH:10][C:7]2[CH:8]=[CH:9][C:4]([O:3][C:2]([F:1])([F:27])[F:28])=[CH:5][CH:6]=2)=[O:26])[CH2:14][CH2:15]1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 49780163HCID 49780163、化合物

生成物 1

HCID 49780164HCID 49780164、化合物収率 89%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Intermediate 41 (2.02 g, 5.0 mmol) was treated with 1M HCl in methanol (35 mL) and refluxed for 3 hours. The solvent was evaporated and the residue diluted with 1N NaOH. The resulting precipitate was removed by filtration and further dried under high vacuum to give intermediate 42 (1.35 g, 89%) as a white solid: Mp 169-173° C. 1H NMR (500 MHz, DMSO-d6) δ 8.49 (s, 1H), 7.46 (d, J=9.0 Hz, 2H), 7.21 (d, J=8.6 Hz, 2H), 6.15 (d, J=7.7 Hz, 1H), 3.55-3.45 (m, 1H), 2.89 (td, J=12.8, 3.5 Hz, 2H), 2.49-2.45 (m, 2H), 2.13 (s, 1H), 1.74 (dd, J=12.4, 2.4 Hz, 2H), 1.21 (dq, J=11.7, 3.7 Hz, 2H). HRMS calculated for C13H16F3N3O2−H+ 302.1117. found (ESI(−), [M−H]) 302.1114.

後処理

  1. temperaturerefluxed for 3 hours
  2. customThe solvent was evaporated
  3. additionthe residue diluted with 1N NaOH
  4. customThe resulting precipitate was removed by filtration
  5. customfurther dried under high vacuum

出典と根拠

ORDレコード
ord-995633b882af43ddaa081473af61d784
出典データセット
uspto-grants-2016_03
特許番号
US09296693B2

反応ノート

読み込み中…