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

Dimethylformamide → HCID 86636026、化合物

HRID 449021
ノート
印刷プレビュー

反応式

HRID 449021 の反応式
[Cl:1][C:2]1[C:3]([CH:8]([NH2:22])[C:9]2[CH:14]=[CH:13][C:12]([O:15][C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)=[CH:11][CH:10]=2)=[N:4][CH:5]=[CH:6][N:7]=1.[CH:23]1([C:29](O)=[O:30])[CH2:28][CH2:27][CH2:26][CH2:25][CH2:24]1.CCN(C(C)C)C(C)C.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.CN(C=O)C>>[Cl:1][C:2]1[C:3]([CH:8]([NH:22][C:29]([CH:23]2[CH2:28][CH2:27][CH2:26][CH2:25][CH2:24]2)=[O:30])[C:9]2[CH:10]=[CH:11][C:12]([O:15][C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)=[CH:13][CH:14]=2)=[N:4][CH:5]=[CH:6][N: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

6

反応物 5

HCID 6228DimethylformamideHCID 7413Cyclohexanecarboxylic acidHCID 81531DiisopropylethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 59341168HCID 59341168、化合物

生成物 1

HCID 86636026HCID 86636026、化合物収率 108.3%

実験手順

In a 10 mL flask were added C-(3-chloropyrazin-2-yl)-C-(4-phenoxyphenyl)-methylamine (110 mg, 0.35 mmol), cyclohexanecarboxylic acid (0.090 g, 0.00070 mol), DIEA (0.55 mL, 0.0032 mol), TBTU (0.17 g, 0.00053 mol) and DMF (5 mL, 0.07 mol) and the reaction mixture is stirred at rt for 10 min. Reaction mixture was stirred at rt over weekend. The reaction mixture was concentrated in vacuo dissolved in DCM and washed with sat. aq NaHCO3 followed by brine. The organics were collected and concentrated in vacuo to give 160 mg of the compound as a yellow solid. Purification by prep TLC in 60% EtOAc:hexanes afforded 110 mg of the title compound as a light yellow solid. Compound was carried on to the next step. MS(ES+): m/z 422.15 (100)[MH+]. HPLC: tR=3.97 min (Open Lynx, polar—5 min).

後処理

  1. customReaction mixture
  2. stirringwas stirred at rt over weekend
  3. concentrationThe reaction mixture was concentrated in vacuo
  4. dissolutiondissolved in DCM
  5. washwashed with sat. aq NaHCO3
  6. customThe organics were collected
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-bb16b44fe5c444ddaa83ef9ba102d59b
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08481733B2

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