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

Methanol → Hydrochloric Acid

HRID 467376
ノート
印刷プレビュー

反応式

HRID 467376 の反応式
[O:1]=[C:2]1[CH:6]([S:7][C:8]2[CH2:9][S:10][C@@H:11]3[C@H:31]([NH:32]C(=O)CC4C=CC=CC=4)[C:30](=[O:42])[N:12]3[C:13]=2[C:14]([O:16][CH:17]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[O:15])[CH2:5][CH2:4][O:3]1.CN1CCOCC1.P(Cl)(Cl)(Cl)(Cl)[Cl:51].CO>ClCCl.O>[NH2:32][C@@H:31]1[C:30](=[O:42])[N:12]2[C:13]([C:14]([O:16][CH:17]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)=[O:15])=[C:8]([S:7][CH:6]3[CH2:5][CH2:4][O:3][C:2]3=[O:1])[CH2:9][S:10][C@H:11]12.[ClH:51]
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

8

反応物 4

HCID 887MethanolHCID 79724-MethylmorpholineHCID 24819Phosphorus pentachlorideHCID 67908892HCID 67908892、化合物

生成物 2

HCID 313Hydrochloric AcidHCID 67908800HCID 67908800、化合物

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 6344Dichloromethane溶媒2 回

反応条件

温度
-20 °C

実験手順

Diphenylmethyl 3-(2-oxotetrahydrofuran-3-ylthio)-7β-phenylacetamidoceph-3-em-4-carboxylate (733 mg) was suspended in dry dichloromethane (10 ml) under an inert atmosphere. The reaction was cooled to -20° C. and treated with N-methylmorpholine (269 μl) followed by a solution of phosphorus pentachloride in dichloromethane (9.5 ml of 40 mgml-1 solution). The now homogeneous solution was stirred at -20° C. for 30 min. Treated with methanol (2.44 ml) and then continued stirring whilst allowing to warm to room temperature. After 30 min. water (3.3 ml) was added and the solution vigorously stirred for a final 30 min. The organic solvent was removed by evaporation in vacuo. The resulting solid was removed from the aqueous phase by filtration and was washed with water and then ether. Drying the solid over phosphorus pentoxide in vacuo gave the crude title compound in the form of its hydrochloride (621 mg). (c) Diphenylmethyl 3-(2-Oxotetrahydrofuran-3-ylthio)-7β-[2-(2-tritylaminothiazol-4-yl)-2-(Z)-methoxyiminoacetamido]ceph-3-em-4-carboxylate.

後処理

  1. stirringcontinued stirring
  2. temperatureto warm to room temperature
  3. stirringthe solution vigorously stirred for a final 30 min
  4. customThe organic solvent was removed by evaporation in vacuo
  5. customThe resulting solid was removed from the aqueous phase by filtration
  6. washwas washed with water
  7. dry with materialDrying the solid over phosphorus pentoxide in vacuo

出典と根拠

ORDレコード
ord-1f8a9e5222a74f599bc6de796b6b3128
出典データセット
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05158946

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