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 → N-(2'-chloro-4'-isothiocyanato-6'-(trifluoromethyl)biphenyl-3-yl)methanesulfonamide

HRID 1048866
ノート
印刷プレビュー

反応式

HRID 1048866 の反応式
[NH2:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[C:5]([C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([NH:18][S:19]([CH3:22])(=[O:21])=[O:20])[CH:13]=2)=[C:4]([Cl:23])[CH:3]=1.C(=O)([O-])[O-].[Ca+2].[C:29](Cl)(Cl)=[S:30].Cl>ClCCl.O>[Cl:23][C:4]1[CH:3]=[C:2]([N:1]=[C:29]=[S:30])[CH:7]=[C:6]([C:8]([F:11])([F:9])[F:10])[C:5]=1[C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([NH:18][S:19]([CH3:22])(=[O:21])=[O:20])[CH:13]=1
参加物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 313Hydrochloric AcidHCID 10040ThiophosgeneHCID 10112Calcium CarbonateHCID 90390781HCID 90390781、化合物

生成物 1

HCID 90390276N-(2'-chloro-4'-isothiocyanato-6'-(trifluoromethyl)biphenyl-3-yl)methanesulfonamide収率 89%

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 6344Dichloromethane溶媒

実験手順

To a cold (0° C.) suspension of N-(4′-amino-2′-chloro-6′-(trifluoromethyl)biphenyl-3-yl)methanesulfonamide (570 mg, 1.56 mmol, Eq: 1.00) and calcium carbonate (313 mg, 3.13 mmol, Eq: 2) in dichloromethane (3.38 ml) and water (3.38 ml) was added thiophosgene (198 mg, 131 μl, 1.72 mmol, Eq: 1.1). The reaction mixture was allowed to warm up to room temperature and was vigorously stirred for 16 h. 1N HCl was added to adjust the pH to ca. 2. The reaction mixture was partitioned between water and ethyl acetate. The organic layer was separated and washed with water then brine and purified on silica gel (column 24 g, dichloromethane/ethyl acetate 1:0 to 85:15) to give 565 mg (89%) of the desired product as a colorless oil.

後処理

  1. customThe reaction mixture was partitioned between water and ethyl acetate
  2. customThe organic layer was separated
  3. washwashed with water
  4. custombrine and purified on silica gel (column 24 g, dichloromethane/ethyl acetate 1:0 to 85:15)

出典と根拠

ORDレコード
ord-0d42599e31154177b813de70230883bd
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09382218B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート