Triethylamine → 4-(4-Iodophenyl)morpholine
反応式
[I:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[CH:4][CH:3]=1.Br[CH2:10][CH2:11][O:12][CH2:13][CH2:14]Br.CCN(CC)CC>CN(C=O)C.CCOC(C)=O>[I:1][C:2]1[CH:8]=[CH:7][C:5]([N:6]2[CH2:14][CH2:13][O:12][CH2:11][CH2:10]2)=[CH:4][CH:3]=1参加物
6
反応条件
- 温度
- 60 °C
実験手順
Methyl 2-N-boc-amino-5-(4-morpholinophenyl)-pent-4-ynoate: 4-Iodoaniline (6.2 g, 28.4 mmol) is taken in 50 mL of DMF in the presence of 8 mL of bromoethyl ether and 10 mL of Et3N and heated to 60° C. for 24 hr. The mixture is then diluted with EtOAc, and washed 3x with dil. NaHCO3, 1x with brine, dried over MgSO4, filtered and evaporated. The residue is then recrystallized from MeOH to give 4.21 g of 4-iodophenylmorpholine as a pale brown solid.
後処理
- washwashed 3x with dil. NaHCO3, 1x with brine
- dry with materialdried over MgSO4
- filtrationfiltered
- customevaporated
- customThe residue is then recrystallized from MeOH
出典と根拠
- ORDレコード
- ord-55cfd07e5a8f49d8af6616f4918f00b1
- 出典データセット
- uspto-grants-2001_03
- 特許番号
- US06197770B1
反応ノート
読み込み中…