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 → 5-(3,3-Dimethyl-but-1-ynyl)-3-[[2-(ethoxy-methyl-phosphinoyl)-ethyl]-(4-methyl-cyclohexanecarbonyl)-amino]-thiophene-2-carboxylic acid

HRID 1614915
ノート
印刷プレビュー

反応式

HRID 1614915 の反応式
C[O:2][C:3]([C:5]1[S:6][C:7]([C:28]#[C:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[CH:8][C:9]=1[N:10]([CH2:20][CH2:21][P:22]([O:25][CH2:26][CH3:27])([CH3:24])=[O:23])[C:11]([CH:13]1[CH2:18][CH2:17][CH:16]([CH3:19])[CH2:15][CH2:14]1)=[O:12])=[O:4].[Li+].[OH-].O.Cl>C1COCC1.CO>[CH3:32][C:30]([CH3:31])([CH3:33])[C:29]#[C:28][C:7]1[S:6][C:5]([C:3]([OH:4])=[O:2])=[C:9]([N:10]([CH2:20][CH2:21][P:22]([O:25][CH2:26][CH3:27])([CH3:24])=[O:23])[C:11]([CH:13]2[CH2:14][CH2:15][CH:16]([CH3:19])[CH2:17][CH2:18]2)=[O:12])[CH:8]=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 962WaterHCID 3939Lithium HydroxideHCID 670337505-(3,3-Dimethyl-but-1-ynyl)-3-[[2-(ethoxy-methyl-phosphinoyl)-ethyl]-(4-methyl-cyclohexanecarbonyl)-amino]-thiophene-2-carboxylic acid methyl ester

生成物 1

HCID 670359145-(3,3-Dimethyl-but-1-ynyl)-3-[[2-(ethoxy-methyl-phosphinoyl)-ethyl]-(4-methyl-cyclohexanecarbonyl)-amino]-thiophene-2-carboxylic acid
収率 69%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

5-(3,3-Dimethyl-but-1-ynyl)-3-[[2-(ethoxy-methyl-phosphinoyl)-ethyl]-(4-methyl-cyclohexanecarbonyl)-amino]-thiophene-2-carboxylic acid methyl ester (251 mg, 0.51 mmol) was dissolved in THF (7.3 mL) and MeOH (7.3 mL). A 1N solution of LiOH in H2O (1.52 mL, 1.52 mmol) was added to the reaction drop-wise at room temperature. The reaction was run at room temperature until complete, as determined by LC/MS. The reaction was cooled in an ice bath and then acidified to pH 3 with 1N HCl. The entire mixture was then evaporated in vacuo and stored under high vacuum overnight. 5-(3,3-Dimethyl-but-1-ynyl)-3-[[2-(ethoxy-methyl-phosphinoyl)-ethyl]-(4-methyl-cyclohexanecarbonyl)-amino]-thiophene-2-carboxylic acid (168 mg, 69%) was isolated from the residue by reverse phase HPLC. MS (m/z): 481.93 [M+H]+; 31P NMR (161.9 MHz, CDCl3): d 56.771, 55.816.

後処理

  1. customwas run at room temperature
  2. temperatureThe reaction was cooled in an ice bath
  3. customThe entire mixture was then evaporated in vacuo
  4. customstored under high vacuum overnight

出典と根拠

ORDレコード
ord-9e6d6ee67b034b9e9911a884880d5e6a
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08765722B2

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