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

Sodium Carbonate → (S)-2-(2-aminophenyl)-7-methoxy-8-(3-(((S)-7-methoxy-2-(4-methoxyphenyl)-5,11-dioxo-10((2-(trimethylsilyl)ethoxy)methyl)-5,10,11,11a-tetrahydro-pyrrolo[2,1-c][1,4]benzodiazepin-8-yl)oxy)propoxy)-10-((2-(trimethylsilyl)ethoxy)methyl)-pyrrolo[2,1-c][1,4]-benzodiazepine-5,11(10H,11aH)-dione

HRID 594185
ノート
印刷プレビュー

反応式

HRID 594185 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH2:10][C@@H:11]3[N:17]([CH:18]=2)[C:16](=[O:19])[C:15]2[CH:20]=[C:21]([O:62][CH3:63])[C:22]([O:24][CH2:25][CH2:26][CH2:27][O:28][C:29]4[C:59]([O:60][CH3:61])=[CH:58][C:32]5[C:33](=[O:57])[N:34]6[CH:49]=[C:48](S(C(F)(F)F)(=O)=O)[CH2:47][C@H:35]6[C:36](=[O:46])[N:37]([CH2:38][O:39][CH2:40][CH2:41][Si:42]([CH3:45])([CH3:44])[CH3:43])[C:31]=5[CH:30]=4)=[CH:23][C:14]=2[N:13]([CH2:64][O:65][CH2:66][CH2:67][Si:68]([CH3:71])([CH3:70])[CH3:69])[C:12]3=[O:72])=[CH:5][CH:4]=1.[NH2:73][C:74]1[CH:79]=[CH:78][CH:77]=[CH:76][C:75]=1B(O)O.C(=O)([O-])[O-].[Na+].[Na+].C(OCC)(=O)C.CCCCCC>C(O)C.C1(C)C=CC=CC=1.O.C(OCC)(=O)C.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[NH2:73][C:74]1[CH:79]=[CH:78][CH:77]=[CH:76][C:75]=1[C:48]1[CH2:47][C@@H:35]2[N:34]([CH:49]=1)[C:33](=[O:57])[C:32]1[CH:58]=[C:59]([O:60][CH3:61])[C:29]([O:28][CH2:27][CH2:26][CH2:25][O:24][C:22]3[C:21]([O:62][CH3:63])=[CH:20][C:15]4[C:16](=[O:19])[N:17]5[CH:18]=[C:9]([C:6]6[CH:5]=[CH:4][C:3]([O:2][CH3:1])=[CH:8][CH:7]=6)[CH2:10][C@H:11]5[C:12](=[O:72])[N:13]([CH2:64][O:65][CH2:66][CH2:67][Si:68]([CH3:69])([CH3:71])[CH3:70])[C:14]=4[CH:23]=3)=[CH:30][C:31]=1[N:37]([CH2:38][O:39][CH2:40][CH2:41][Si:42]([CH3:43])([CH3:44])[CH3:45])[C:36]2=[O:46]
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

10

反応物 4

HCID 10340Sodium CarbonateHCID 2773216(2-Aminophenyl)boronic acidHCID 21226206Ethyl acetate hexaneHCID 86676188HCID 86676188、化合物

生成物 1

HCID 86676192
(S)-2-(2-aminophenyl)-7-methoxy-8-(3-(((S)-7-methoxy-2-(4-methoxyphenyl)-5,11-dioxo-10((2-(trimethylsilyl)ethoxy)methyl)-5,10,11,11a-tetrahydro-pyrrolo[2,1-c][1,4]benzodiazepin-8-yl)oxy)propoxy)-10-((2-(trimethylsilyl)ethoxy)methyl)-pyrrolo[2,1-c][1,4]-benzodiazepine-5,11(10H,11aH)-dione
収率 90.3%

試薬・触媒・溶媒 5

HCID 178418397HCID 178418397、化合物触媒HCID 702Ethanol溶媒HCID 962Water溶媒HCID 1140Toluene溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
40 °C

実験手順

A catalytic amount of tetrakistriphenylphosphinepalladium (0) (11.2 mg) was added to a mixture of the mono triflate 17 (380 mg), the pinnacol ester of 2-aminophenylboronic acid (124 mg) and sodium carbonate (120 mg) in ethanol (5 mL), toluene (5 mL) and water (5 mL). The reaction mixture was allowed to stir over night at room temperature and at 40° C. until the reaction was complete (c. 2 hr). The reaction mixture was diluted with ethyl acetate and the organic layer was washed with water and brine. The ethyl acetate solution was dried over magnesium sulphate and filtered under vacuum. Removal of ethyl acetate by rotary evaporation under reduced pressure afforded the crude product which was subjected to flash chromatography (silica gel, ethyl acetate/hexane). Pure fractions were collected and combined. Removal of excess eluent by rotary evaporation under reduced pressure afforded the pure product 103 (330 mg, 86% yield). LC/MS RT: 4.17 min, ES+1018.48.

後処理

  1. custom(c. 2 hr)
  2. washthe organic layer was washed with water and brine
  3. dry with materialThe ethyl acetate solution was dried over magnesium sulphate
  4. filtrationfiltered under vacuum
  5. customRemoval of ethyl acetate
  6. customby rotary evaporation under reduced pressure
  7. customafforded the crude product which
  8. customPure fractions were collected
  9. customRemoval of excess eluent
  10. customby rotary evaporation under reduced pressure

出典と根拠

ORDレコード
ord-a92c967aabcf4731b4bdbaf5618861cb
出典データセット
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09242013B2

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