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

Hydrochloric Acid → HCID 20350647、化合物

HRID 1449236
ノート
印刷プレビュー

反応式

HRID 1449236 の反応式
[CH2:1]([N:8]([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=1[CH:23]=[C:24]([S:27](C)=O)SC)[C:9]1[C:14]([Cl:15])=[CH:13][CH:12]=[CH:11][C:10]=1[Cl:16])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.C(Cl)Cl.[OH2:34].[CH3:35][O:36][CH2:37][CH2:38][O:39]C>>[CH2:1]([N:8]([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=1[CH2:37][C:38]([OH:39])=[O:34])[C:9]1[C:10]([Cl:16])=[CH:11][CH:12]=[CH:13][C:14]=1[Cl:15])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:1]([N:8]([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=1[CH2:23][C:24]([O:36][CH3:35])=[S:27])[C:9]1[C:14]([Cl:15])=[CH:13][CH:12]=[CH:11][C:10]=1[Cl:16])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
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 5

HCID 313Hydrochloric AcidHCID 962WaterHCID 6344DichloromethaneHCID 80711,2-DimethoxyethaneHCID 54175266HCID 54175266、化合物

生成物 2

HCID 13023173HCID 13023173、化合物収率 14%HCID 20350647
HCID 20350647、化合物
収率 81%

反応条件

温度
80 °C

実験手順

In 26 ml of 1,2-dimethoxyethane, 1.2 g (0.0026 mole) of 1-[N-benzyl-o-(2,6-dichloroanilino)phenyl]-2-methylsulfinyl-2-methylthioethylene was dissolved and then, 13 ml of conc. HCl was added and the mixture was stirred at 80° C. for 4 hours. The reaction mixture was cooled and 80 ml of methylene chloride and 10 ml of water were added to extract the reaction product and the separated water phase was further mixed with 70 ml of methylene chloride to extract the reaction product. Both of methylene chloride phases were combined, dried over anhydrous sodium sulfate, and then concentrated under reduced pressure. The residue was separated by a column chromatography (silica gel: Wako gel Q-23 manufactured by Wako Junyaku and developing solvent:n-hexane:acetone=2:1) to obtain 0.14 g (yield: 14%) of N-benzyl-o-(2,6-dichloroanilino)phenyl acetic acid and 0.88 g (yield: 81%) of methyl N-benzyl-o-(2,6-dichloroanilino)phenylthioacetate.

後処理

  1. temperatureThe reaction mixture was cooled
  2. extractionto extract the reaction product
  3. additionthe separated water phase was further mixed with 70 ml of methylene chloride
  4. extractionto extract the reaction product
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was separated by a column chromatography (silica gel: Wako gel Q-23 manufactured by Wako Junyaku and developing solvent:n-hexane:acetone=2:1)

出典と根拠

ORDレコード
ord-ddffbd3595b24f63825b6be4d2dae32e
出典データセット
uspto-grants-1980_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04189595

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