tert-butyl 9-(2-methylpropa-1-ene-1-yl)-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate → tert-butyl 9-(2-methylpropyl)-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate

HRID 886940ノート

反応式

HRID 886940 の反応式
[CH3:1][C:2]([CH3:22])=[CH:3][C:4]1[C:14]2[O:13][CH2:12][CH2:11][N:10]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:9][C:8]=2[CH:7]=[CH:6][CH:5]=1>[Pd].CO>[CH3:1][CH:2]([CH3:22])[CH2:3][C:4]1[C:14]2[O:13][CH2:12][CH2:11][N:10]([C:15]([O:17][C:18]([CH3:19])([CH3:21])[CH3:20])=[O:16])[CH2:9][C:8]=2[CH:7]=[CH:6][CH:5]=1

参加物

4

反応物 1

HCID 68580669tert-butyl 9-(2-methylpropa-1-ene-1-yl)-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate

生成物 1

HCID 68579404tert-butyl 9-(2-methylpropyl)-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate収率 95.7%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

A solution of tert-butyl 9-(2-methylpropa-1-ene-1-yl)-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate (270 mg, 0.890 mmol) and 10% palladium on carbon (50.0 mg) in methanol (6 ml) was stirred under a hydrogen atmosphere for 12 hr. The reaction mixture was filtered, and the filtrate was concentrated. The residue was poured into water, and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure to give the desired product (260 mg, 95.6%) as an oil.

後処理

  1. filtrationThe reaction mixture was filtered
  2. concentrationthe filtrate was concentrated
  3. additionThe residue was poured into water
  4. extractionthe mixture was extracted with ethyl acetate
  5. dry with materialThe extract was dried over anhydrous magnesium sulfate
  6. customthe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-cdb1fb7738804feeba1cc71fb2065fd8
出典データセット
uspto-grants-2012_08
特許番号
US08247403B2

反応ノート

読み込み中…