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 Hydroxide → HCID 66849728、化合物

HRID 1046433
ノート
印刷プレビュー

反応式

HRID 1046433 の反応式
[H-].[Na+:2].C[O:4][C:5]([C:7]1[S:8][C:9]([C:29]#[C:30][C:31]([CH3:34])([CH3:33])[CH3:32])=[CH:10][C:11]=1[N:12]([CH:22]1[CH2:27][CH2:26][CH:25]([OH:28])[CH2:24][CH2:23]1)[C:13]([CH:15]1[CH2:20][CH2:19][CH:18]([CH3:21])[CH2:17][CH2:16]1)=[O:14])=[O:6].F[C:36]1[CH:41]=[C:40]([CH2:42][N:43]([CH3:45])[CH3:44])[CH:39]=[CH:38][N:37]=1.[OH-].[Na+]>CN(C=O)C>[CH3:44][N:43]([CH2:42][C:40]1[CH:39]=[CH:38][N:37]=[C:36]([O:28][CH:25]2[CH2:26][CH2:27][CH:22]([N:12]([C:11]3[CH:10]=[C:9]([C:29]#[C:30][C:31]([CH3:32])([CH3:33])[CH3:34])[S:8][C:7]=3[C:5]([O-:4])=[O:6])[C:13]([CH:15]3[CH2:20][CH2:19][CH:18]([CH3:21])[CH2:17][CH2:16]3)=[O:14])[CH2:23][CH2:24]2)[CH:41]=1)[CH3:45].[Na+:2]
参加物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 14798Sodium HydroxideHCID 24758Sodium hydrideHCID 58113973HCID 58113973、化合物HCID 581139915-(3,3-Dimethyl-but-1-ynyl)-3-[(4-hydroxy-cyclohexyl)-(4-methyl-cyclohexanecarbonyl)-amino]-thiophene-2-carboxylic acid methyl ester

生成物 1

HCID 66849728HCID 66849728、化合物収率 31%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

NaH (65 mg of a 60% oil dispersion, 1.62 mmol) was added to solution 5-(3,3-dimethyl-but-1-ynyl)-3-[(4-hydroxy-cyclohexyl)-(4-methyl-cyclohexanecarbonyl)-amino]-thiophene-2-carboxylic acid methyl ester (155 mg, 0.34 mmol) and (2-fluoro-pyridin-4-ylmethyl)-dimethyl-amine (130 mg, 0.84 mmol) in DMF (4.0 mL) at 0° C. After 5 min the reaction was warmed to room temperature and then heated at 65° C. for 2 h. The reaction was cooled, aqueous NaOH (0.5 mL of a 1.0 N solution) was added and the reaction mixture evaporated to dryness. Purification by column chromatography on reverse phase C18 silica gel (100% water to 20% acetonitrile/water) provided the desired product as a colorless solid (62 mg, 31%) after lyophilization. MS (m/z): 580.2 [M+H]; HPLC retention time: 5.05 min (2-98% acetonitrile:water with 0.05% trifluoroacetic acid).

後処理

  1. temperatureheated at 65° C. for 2 h
  2. temperatureThe reaction was cooled
  3. customthe reaction mixture evaporated to dryness
  4. customPurification by column chromatography on reverse phase C18 silica gel (100% water to 20% acetonitrile/water)

出典と根拠

ORDレコード
ord-938cfbca17674452bc91b58c0a15ff70
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08569302B2

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