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

Triethylamine → (S)-Methyl 2-(3-(4-(3-(2-fluorophenyl)ureido)phenyl)isoxazole-5-carboxamido)-3-hydroxypropanoate

HRID 75832
ノート
印刷プレビュー

反応式

HRID 75832 の反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH:8][C:9](=[O:25])[NH:10][C:11]1[CH:16]=[CH:15][C:14]([C:17]2[CH:21]=[C:20]([C:22](O)=[O:23])[O:19][N:18]=2)=[CH:13][CH:12]=1.C1(N=C=NC2CCCCC2)CCCCC1.ON1C2C=CC=CC=2N=N1.Cl.[CH3:52][O:53][C:54](=[O:59])[C@H:55]([CH2:57][OH:58])[NH2:56].C(N(CC)CC)C>CN(C=O)C.C1COCC1>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH:8][C:9](=[O:25])[NH:10][C:11]1[CH:12]=[CH:13][C:14]([C:17]2[CH:21]=[C:20]([C:22]([NH:56][C@@H:55]([CH2:57][OH:58])[C:54]([O:53][CH3:52])=[O:59])=[O:23])[O:19][N:18]=2)=[CH:15][CH:16]=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 5

HCID 8471TriethylamineHCID 10868DicyclohexylcarbodiimideHCID 757711-HydroxybenzotriazoleHCID 2723730L-Serine, methyl ester, hydrochloride (1:1)HCID 673539813-(4-(3-(2-Fluorophenyl)ureido)phenyl)isoxazole-5-carboxylic acid

生成物 1

HCID 67352794
(S)-Methyl 2-(3-(4-(3-(2-fluorophenyl)ureido)phenyl)isoxazole-5-carboxamido)-3-hydroxypropanoate
収率 39%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

3-(4-(3-(2-fluorophenyl)ureido)phenyl)isoxazole-5-carboxylic acid (example 105, step 2, 1 g, 293 mmol) was dissolved in DMF (20 ml) and, to it N,N′-Dicyclohexyl carbodiimide (724 mg, 3.51 mmol) and 1-Hydroxy benzotriazole (593 mg, 4.39 mmol) were added. Reaction mixture was stirred RT for 10 minutes followed by the addition of L-serine methyl ester hydrochloride (683 mg, 4.39 mmol) dissolved in DMF (5 ml) neutralized with triethylamine (0.6 ml, 4.39 mmol). The above reaction mixture was stirred at RT for 8 hours. DMF was distilled off under reduced pressure to give pale brown solid, which was taken in THF. DCU precipitated out and was filtered off. Water was added and the aqueous layer was extracted with EtOAc. Organic layer was dried over Na2SO4 and concentrated under vacuum. Crude compound was purified through precipitation using DCM and petroleum ether to yield 500 mg (39%) of the required compound as white solid. MS: ES (−): m/z 441(M−1); ES (+): m/z 443 (M+1); 1HNMR (DMSO-d6; 300 MHz): δ 9.342 (s, 1H), 9.109 (d; 1H), 8.633 (s, 1H), 8.161 (t, 1H), 7.369 (d, 2H), 7.676 (s, 1H), 7.619 (d, 2H), 7.242 (m, 1H), 7.066 (t, 1H), 7.024 (m, 1H), 5.149 (t, 1H), 4.575 (m, 1H), 3.821 (t, 2H), 3.657 (s, 3H).

後処理

  1. additionwere added
  2. customReaction mixture
  3. customThe above reaction mixture
  4. stirringwas stirred at RT for 8 hours
  5. distillationDMF was distilled off under reduced pressure
  6. customto give pale brown solid, which
  7. customDCU precipitated out
  8. filtrationwas filtered off
  9. additionWater was added
  10. extractionthe aqueous layer was extracted with EtOAc
  11. dry with materialOrganic layer was dried over Na2SO4
  12. concentrationconcentrated under vacuum
  13. customCrude compound was purified through precipitation

出典と根拠

ORDレコード
ord-34efe286c4624832b702390bc7862409
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08835428B2

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