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-Hydroxybenzotriazole → 2-(4-Fluoro-phenylsulfanyl)-N-trityloxy-acetamide

HRID 1716318
ノート
印刷プレビュー

反応式

HRID 1716318 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][CH2:9][C:10]([OH:12])=O)=[CH:4][CH:3]=1.[C:13]([O:32][NH2:33])([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.CCN=C=NCCCN(C)C.Cl.C1C=CC2N(O)N=NC=2C=1>CN(C=O)C.CCOC(C)=O.O.CN1C(=O)CCC1>[F:1][C:2]1[CH:3]=[CH:4][C:5]([S:8][CH2:9][C:10]([NH:33][O:32][C:13]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)([C:26]2[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=2)[C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)=[O:12])=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

HCID 757711-HydroxybenzotriazoleHCID 7361972-[(4-Fluorophenyl)sulfanyl]acetic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 3015602O-(triphenylmethyl)hydroxylamine

生成物 1

HCID 866199392-(4-Fluoro-phenylsulfanyl)-N-trityloxy-acetamide

試薬・触媒・溶媒 4

HCID 962
Water
溶媒
HCID 6228Dimethylformamide溶媒
HCID 8857Ethyl Acetate溶媒
HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

A mixture of (4-fluoro-phenylsulfanyl)-acetic acid (1.52 g, 8.17 mmol) from step B and O-Trityl-hydroxylamine (2.26 g, 10 mmol) in dry DMF was sequentially added NMP (3.0 ml), EDCl (2.05 g, 10.7 mmol), and HOBT (1.45 g, 10.74 mmol). The resulting mixture was stirred at room temperature for overnight. The reaction was diluted with EtOAc and water. The organic layer was washed sequentially with 1N HCl solution, 10% aqueous Na2CO3, water and saturated NaCl solution. The organic portion was dried over anhydrous Na2SO4 and concentrated under reduced pressure to gave a crude material, which was then purified by a column chromatography with 0˜25% EtOAc in hexanes. MS: 466.0 (M+H)+.

後処理

  1. washThe organic layer was washed sequentially with 1N HCl solution, 10% aqueous Na2CO3, water and saturated NaCl solution
  2. dry with materialThe organic portion was dried over anhydrous Na2SO4
  3. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-a60109d474054772818a90f4820ddbdc
出典データセット
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07803793B2

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