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

1,2-Dichloroethane → HCID 58011813、化合物

HRID 660940
ノート
印刷プレビュー

反応式

HRID 660940 の反応式
[Cl:1][C:2]1[S:6][C:5]([C:7]2[N:11]([CH2:12][C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[F:19])[C:10](=[O:20])[N:9]([CH2:21][C:22]([OH:24])=O)[N:8]=2)=[CH:4][CH:3]=1.[F:25][C:26]([F:38])([F:37])[C:27]1[CH:28]=[C:29]([C:33]([NH2:36])([CH3:35])[CH3:34])[CH:30]=[CH:31][CH:32]=1.C1C=CC2N(O)N=NC=2C=1.C(Cl)CCl>CN(C=O)C.C(OCC)(=O)C.O>[Cl:1][C:2]1[S:6][C:5]([C:7]2[N:11]([CH2:12][C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[F:19])[C:10](=[O:20])[N:9]([CH2:21][C:22]([NH:36][C:33]([CH3:35])([C:29]3[CH:30]=[CH:31][CH:32]=[C:27]([C:26]([F:25])([F:37])[F:38])[CH:28]=3)[CH3:34])=[O:24])[N:8]=2)=[CH:4][CH:3]=1
参加物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 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 194252732-[3-(Trifluoromethyl)phenyl]propan-2-amineHCID 58011885HCID 58011885、化合物

生成物 1

HCID 58011813HCID 58011813、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒
HCID 6228
Dimethylformamide
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

The carboxylic acid from Example 154A (150 mg, 0.41 mmol) and 1-methyl-1-(3-trifluoromethyl-phenyl)ethylamine (Example 1A, 91.2 mg, 0.45 mmol) are placed in 4 ml DMF and treated at RT with 66.1 mg (0.49 mmol) of HOBt. After 10 mins, 101.6 mg (0.53 mmol) of EDC are added and the mixture stirred overnight at RT. It is then treated with water and ethyl acetate. The phases are separated, and the aqueous phase is extracted with ethyl acetate. The combined organic phases are washed with water, then with sat. sodium chloride solution, dried by filtration through an Extrelut cartridge and freed of the volatile components on the rotary evaporator. The residue is purified by chromatography on silica gel (Biotage cartridge 25M, eluent: cyclohexane/ethyl acetate 1:1). 192 mg (85% of theory) of the title compound are thus obtained.

後処理

  1. customThe phases are separated
  2. extractionthe aqueous phase is extracted with ethyl acetate
  3. washThe combined organic phases are washed with water
  4. dry with materialwith sat. sodium chloride solution, dried by filtration through an Extrelut cartridge
  5. customfreed of the volatile components on the rotary evaporator
  6. customThe residue is purified by chromatography on silica gel (Biotage cartridge 25M, eluent: cyclohexane/ethyl acetate 1:1)

出典と根拠

ORDレコード
ord-466cd7eb923a4ec0aab95bd63db61485
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08084481B2

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