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 → (R)-4-cyano-3-hydroxybutyric acid

HRID 2079451
ノート
印刷プレビュー

反応式

HRID 2079451 の反応式
[OH:1][CH:2](CC#N)[CH2:3][C:4]#[N:5].CC[O:11][C:12]([CH3:14])=[O:13].Cl>N#N>[OH:1][C@H:2]([CH2:3][C:4]#[N:5])[CH2:14][C:12]([OH:11])=[O:13]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 3617621,3-Dicyano-2-propanol

生成物 1

HCID 10236005(R)-4-cyano-3-hydroxybutyric acid

試薬・触媒・溶媒 1

HCID 947Nitrogen溶媒

実験手順

3-hydroxyglutaronitrile (1 g, 9 mmol) was suspended in 37.5 mL of N2 (g) sparged, room temperature, 100 mM sodium phosphate buffer at pH 7. To this 240 mM solution of HGN was added 150 mg of cell lysate normalized for protein content. As assessed by PAGE, the nitrilase content was established to be 20% of the total protein. Therefore effectively, 30 mg of nitrilase is used in this reaction. The reaction was agitated at 100 rpm. Reaction progress was monitored by TLC (1:1 EtOAc:Hexanes, Rf=0.32, nitrile; Rf=0.0, acid) and GC. After 22 h, the reaction was filtered through a 10,000 MW cutoff filter and then concentrated in vacuo. The concentrated hydrolysis solution was acidified with 1M HCl and the product was continuously extracted with MTBE (30 mL). The acid product (R)-3-hydroxy-4-cyanobutyric acid was isolated as a yellow oil (1.15 g, 98% yield). 1H NMR (d6-DMSO, 500 MHz) δ12.32 (s, 1H), 5.52 (s, 1H), 4.10 (m, 1H), 2.70 (dd, 1H, J=16.8, 4.1 Hz), 2.61 (dd, 1H, J=16.9, 6.3 Hz), 2.44 (dd, 1H, J=15.4, 5.3 Hz), 2.37 (dd, 1H, J=15.6, 7.8 Hz). 13C NMR (DMSO, 298K, 125 MHz) δ171.9, 118.7, 63.4, 41.2, 25.2 MS calc'd for [C5H7NO3]: 129.0, found: 130.0 [M+H+], (ESI+). ee=95% [HPLC]. Based on the isolated yield a productivity of 40 g g−1 d−1 is calculated.

後処理

  1. customsparged, room temperature
  2. additionTo this 240 mM solution of HGN was added 150 mg of cell lysate
  3. customTherefore effectively, 30 mg of nitrilase is used in this reaction
  4. customReaction progress
  5. filtrationthe reaction was filtered through a 10,000 MW cutoff
  6. filtrationfilter
  7. concentrationconcentrated in vacuo
  8. customThe concentrated hydrolysis solution
  9. extractionthe product was continuously extracted with MTBE (30 mL)

出典と根拠

ORDレコード
ord-ce68bc9b8b1343708d1a0c229c5a8f0f
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07932064B2

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