1,4-Dioxane → HCID 178441228、化合物

HRID 406280ノート

反応式

HRID 406280 の反応式
CC([N:5]([C@H:9]1[CH2:12][C@H:11]([O:13][C:14]2[CH:19]=[C:18]([F:20])[C:17]([C:21]([CH3:24])([CH3:23])[CH3:22])=[C:16]([F:25])[CH:15]=2)[CH2:10]1)C(=O)[O-])(C)C.O1CCOCC1>Cl>[CH3:24][C:21]([C:17]1[C:16]([F:25])=[CH:15][C:14]([O:13][C@H:11]2[CH2:10][C@H:9]([NH2:5])[CH2:12]2)=[CH:19][C:18]=1[F:20])([CH3:22])[CH3:23]

参加物

4

反応物 2

HCID 312751,4-DioxaneHCID 178441233HCID 178441233、化合物

生成物 1

HCID 178441228HCID 178441228、化合物収率 77.1%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

1,1-dimethylethyl(trans-3-{[4-(1,1-dimethylethyl)-3,5-difluorophenyl]oxy}cyclobutyl)carbamate (257 mg, 0.723 mmol) was stirred in 4M HCl in dioxane (5 mL, 20 mmol) overnight and then concentrated in vacuo and loaded onto an SCX cartridge (10 g) and eluted with MeOH (3 column volumes) and then flushed with ammonia in MeOH. Concentration of the product containing fractions in vacuo gave the title compound (142.3 mg).

後処理

  1. concentrationconcentrated in vacuo
  2. washeluted with MeOH (3 column volumes)
  3. customflushed with ammonia in MeOH
  4. additionConcentration of the product containing fractions in vacuo

出典と根拠

ORDレコード
ord-77cc67c5070c4109934745d28da33a67
出典データセット
uspto-grants-2014_06
特許番号
US08754101B2

反応ノート

読み込み中…