ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

4-Methylmorpholine → HCID 69352349、化合物

HRID 1281078
ノート
印刷プレビュー

反応式

HRID 1281078 の反応式
[NH:1]1[CH:8]=[C:7]([CH2:9][C:10]([OH:12])=O)[C:5](=[O:6])[NH:4][C:2]1=[O:3].CN1CCOCC1.[C:20]([CH:27]([NH2:36])[CH2:28][NH:29][CH2:30][C:31]([O:33][CH2:34][CH3:35])=[O:32])([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21].F[B-](F)(F)F.O=C1C2C=CC=CC=2N=NN1OC(N(C)C)=[N+](C)C>C(OCC)(=O)C.CN(C=O)C>[C:20]([CH:27]([NH2:36])[CH2:28][N:29]([C:10](=[O:12])[CH2:9][C:7]1[C:5](=[O:6])[NH:4][C:2](=[O:3])[NH:1][CH:8]=1)[CH2:30][C:31]([O:33][CH2:34][CH3:35])=[O:32])([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 79724-MethylmorpholineHCID 298035Uracil-5-ylacetic acidHCID 10882602O-(3,4-Dihydro-4-oxo-1,2,3-benzotriazin-3-yl)-N,N,N',N'-tetramethyluronium TetrafluoroborateHCID 57253309HCID 57253309、化合物

生成物 1

HCID 69352349HCID 69352349、化合物

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
0 °C

実験手順

Uracil-5-ylacetic acid (34, 1.0 g, 5.9 mmol) was transferred to a round bottomed flask equipped with a septum through which a flow of nitrogen was applied. Dry DMF (10 ml) and N-methylmorpholine (1.9 ml, 17.6 mmol) were transferred to the flask and the mixture was cooled to 0° C. Ethyl N-(2-BOC-aminoethyl)glycinate (1.6 g, 6.5 mmol) and O-(3,4-dihydro-4-oxo-1,2,3-benzotriazin-3-yl)-N,N,N′,N′-tetramethyl uronium tetrafluoroborate (TDBTU, 2.5 g, 7.0 mmol) were added to the mixture. The reaction mixture was stirred for 3 hours at 0° C. and was then poured into ethyl acetate (300 ml). The resultant suspension was washed with saturated aqueous potassium hydrogen sulfate (2×50 ml), saturated aqueous sodium bicarbonate (2×50 ml) and with brine (1×50 ml). The organic phase was dried over magnesium sulfate, filtered and evaporated under reduced pressure. The residue was stirred overnight in dichloromethane (10 ml) and diethyl ether (40 ml). The resultant precipitate was isolated by filtration, washed once with diethyl ether and dried to give 1.13 g (48%) of the title compound as white crystals.

後処理

  1. customequipped with a septum through which a flow of nitrogen
  2. washThe resultant suspension was washed with saturated aqueous potassium hydrogen sulfate (2×50 ml), saturated aqueous sodium bicarbonate (2×50 ml) and with brine (1×50 ml)
  3. dry with materialThe organic phase was dried over magnesium sulfate
  4. filtrationfiltered
  5. customevaporated under reduced pressure
  6. stirringThe residue was stirred overnight in dichloromethane (10 ml)

出典と根拠

ORDレコード
ord-4cf3c53ac1584698ab8fe1af89e4eec7
出典データセット
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06451968B1

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート