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

Lithium Hydroxide → HCID 90418710、化合物

HRID 2177195
ノート
印刷プレビュー

反応式

HRID 2177195 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH2:28][CH2:29][C:30]([O:32]CC)=[O:31])[CH:5]=[C:6]([F:27])[C:7]=1[O:8][CH2:9][C:10]1[C:11]([C:19]2[CH:20]=[N:21][C:22]([O:25][CH3:26])=[CH:23][CH:24]=2)=[N:12][S:13][C:14]=1[C:15]([F:18])([F:17])[F:16].COC1C=CC(C(N)=O)=CN=1.O1CCCC1.[Li+].[OH-]>O>[F:1][C:2]1[CH:3]=[C:4]([CH2:28][CH2:29][C:30]([OH:32])=[O:31])[CH:5]=[C:6]([F:27])[C:7]=1[O:8][CH2:9][C:10]1[C:11]([C:19]2[CH:20]=[N:21][C:22]([O:25][CH3:26])=[CH:23][CH:24]=2)=[N:12][S:13][C:14]=1[C:15]([F:16])([F:17])[F:18]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 2508106-MethoxynicotinamideHCID 90418756HCID 90418756、化合物

生成物 1

HCID 90418710HCID 90418710、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
20 °C

実験手順

Into a 25-mL round-bottom flask, was placed ethyl 3-(3,5-difluoro-4-[[3-(6-methoxypyridin-3-yl)-5-(trifluoromethyl)-1,2-thiazol-4-yl]methoxy]phenyl)propanoate (prepared according to the procedure following Example 1 step 1-5 using 6-methoxynicotinamide as starting material) (50 mg, 0.10 mmol, 1.00 equiv), tetrahydrofuran (1 mL), LiOH (50 mg, 2.09 mmol, 20.98 equiv), water (1 mL). The resulting solution was stirred overnight at 20° C. The resulting mixture was concentrated under vacuum. The pH value of the solution was adjusted to 6 with hydrogen chloride (2 mol/L). The solids were collected by filtration. The crude product (20 mg) was purified by Flash-Prep-HPLC with the following conditions (IntelFlash-1): Reversed Column, C18 silica gel; mobile phase, 0.05% TFA/ACN=1/4 increasing to 0.05% TFA/ACN=0/1 within 20 min; Detector, UV 254 nm. This resulted in 8.8 mg (18%) of 3-(3,5-difluoro-4-((3-(6-methoxypyridin-3-yl)-5-(trifluoromethyl)isothiazol-4-yl)methoxy)phenyl)propanoic acid as a white solid. 1H NMR (300 MHz, CD3OD) δ 8.51 (s, 1H), 8.06 (d, J=6.3 Hz, 1H), 6.80-6.89 (m, 3H), 5.19 (s, 2H), 3.96 (s, 3H), 2.83 (t, J=7.5 Hz, 2H), 2.56 (t, J=7.5 Hz, 2H). Mass spectrum (ESI, m/z): Calcd. for C20H15F5N2O4S, 475.1 (M+H). found 475.1.

後処理

  1. customInto a 25-mL round-bottom flask, was placed
  2. concentrationThe resulting mixture was concentrated under vacuum
  3. filtrationThe solids were collected by filtration
  4. customThe crude product (20 mg) was purified by Flash-Prep-HPLC with the following conditions (IntelFlash-1)
  5. waitmobile phase, 0.05% TFA/ACN=1/4 increasing to 0.05% TFA/ACN=0/1 within 20 min
  6. customThis resulted in 8.8 mg (18%) of 3-(3,5-difluoro-4-((3-(6-methoxypyridin-3-yl)-5-(trifluoromethyl)isothiazol-4-yl)methoxy)phenyl)propanoic acid as a white solid

出典と根拠

ORDレコード
ord-d9241b2a0005405e8eb2b23adcb38ec7
出典データセット
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09067898B1

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート