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

Acetic Acid → (R)-5-(1-(tert-Butyldimethylsilyloxy)-2-(3-(3-(4-(2-methylthiazole-4-carbonyl)-1-oxa-4,9-diazaspiro[5.5]undecan-9-yl)propoxy)benzylamino)ethyl)-8-hydroxyquinolin-2(1H)-one

HRID 1689453
ノート
印刷プレビュー

反応式

HRID 1689453 の反応式
C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].[CH3:15][C:16]1[S:17][CH:18]=[C:19]([C:21]([N:23]2[CH2:28][C:27]3([CH2:33][CH2:32][N:31]([CH2:34][CH2:35][CH2:36][O:37][C:38]4[CH:39]=[C:40]([CH:43]=[CH:44][CH:45]=4)[CH:41]=O)[CH2:30][CH2:29]3)[O:26][CH2:25][CH2:24]2)=[O:22])[N:20]=1.[NH2:46][CH2:47][C@@H:48]([C:57]1[CH:66]=[CH:65][C:64]([OH:67])=[C:63]2[C:58]=1[CH:59]=[CH:60][C:61](=[O:68])[NH:62]2)[O:49][Si:50]([C:53]([CH3:56])([CH3:55])[CH3:54])([CH3:52])[CH3:51].C(O)(=O)C>CO>[Si:50]([O:49][C@H:48]([C:57]1[CH:66]=[CH:65][C:64]([OH:67])=[C:63]2[C:58]=1[CH:59]=[CH:60][C:61](=[O:68])[NH:62]2)[CH2:47][NH:46][CH2:41][C:40]1[CH:43]=[CH:44][CH:45]=[C:38]([O:37][CH2:36][CH2:35][CH2:34][N:31]2[CH2:32][CH2:33][C:27]3([O:26][CH2:25][CH2:24][N:23]([C:21]([C:19]4[N:20]=[C:16]([CH3:15])[S:17][CH:18]=4)=[O:22])[CH2:28]3)[CH2:29][CH2:30]2)[CH:39]=1)([C:53]([CH3:56])([CH3:55])[CH3:54])([CH3:52])[CH3:51]
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 176Acetic AcidHCID 5049666Sodium triacetoxyborohydrideHCID 579889423-(3-(4-(2-Methylthiazole-4-carbonyl)-1-oxa-4,9-diazaspiro[5.5]undecan-9-yl)propoxy)benzaldehydeHCID 59023604(R)-5-(2-Amino-1-((tert-butyldimethylsilyl)oxy)ethyl)-8-hydroxyquinolin-2(1H)-one

生成物 1

HCID 67292255
(R)-5-(1-(tert-Butyldimethylsilyloxy)-2-(3-(3-(4-(2-methylthiazole-4-carbonyl)-1-oxa-4,9-diazaspiro[5.5]undecan-9-yl)propoxy)benzylamino)ethyl)-8-hydroxyquinolin-2(1H)-one

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
20 °C

実験手順

Sodium triacetoxyborohydride (0.113 g) was added in one portion to a stirred solution at 0° C. of 3-(3-(4-(2-methylthiazole-4-carbonyl)-1-oxa-4,9-diazaspiro[5.5]undecan-9-yl)propoxy)benzaldehyde (example 95, step b) (0.157 g), (R)-5-(2-amino-1-(tert-butyldimethylsilyloxy)ethyl)-8-hydroxyquinolin-2(1H)-one (WO2004106333) (0.118 g) and acetic acid (0.020 mL) in methanol (7 mL). The resulting mixture was stirred at 20° C. for 2 hours. Most of the methanol was evaporated under reduced pressure and the residue was partitioned between ethyl acetate and aqueous phosphate buffer (pH=7.2), the organic layer was dried over sodium sulphate, filtered and the solvent evaporated under reduced pressure. The crude product was purified by flash silica chromatography using 8% methanol and 1% ‘880’ aqueous ammonia in dichloromethane as solvent. Pure fractions were evaporated to dryness to afford the subtitled compound. Yield 0.160 g.

後処理

  1. customMost of the methanol was evaporated under reduced pressure
  2. customthe residue was partitioned between ethyl acetate and aqueous phosphate buffer (pH=7.2)
  3. dry with materialthe organic layer was dried over sodium sulphate
  4. filtrationfiltered
  5. customthe solvent evaporated under reduced pressure
  6. customThe crude product was purified by flash silica chromatography
  7. customPure fractions were evaporated to dryness

出典と根拠

ORDレコード
ord-09ceb3289b27427fb70b9a0962c14195
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08148373B2

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