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

Diisopropylethylamine → [5-(2-Chloro-6-methyl-pyridin-4-yl)-3-(2,2-difluoro-benzo[1,3]dioxol-5-ylamino)-[1,2,4]triazol-1-yl]acetic acid ethyl ester

HRID 1952183
ノート
印刷プレビュー

反応式

HRID 1952183 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:23]=[C:24]([CH3:26])[N:25]=1)[C:5]([NH:7][CH:8]([NH:11][C:12]1[CH:22]=[CH:21][C:15]2[O:16][C:17]([F:20])([F:19])[O:18][C:14]=2[CH:13]=1)SC)=O.Cl.[CH2:28]([O:30][C:31](=[O:35])[CH2:32][NH:33][NH2:34])[CH3:29].C(N(C(C)C)C(C)C)C>CC(O)(C)C>[CH2:28]([O:30][C:31](=[O:35])[CH2:32][N:33]1[C:5]([C:4]2[CH:23]=[C:24]([CH3:26])[N:25]=[C:2]([Cl:1])[CH:3]=2)=[N:7][C:8]([NH:11][C:12]2[CH:22]=[CH:21][C:15]3[O:16][C:17]([F:20])([F:19])[O:18][C:14]=3[CH:13]=2)=[N:34]1)[CH3:29]
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

5

反応物 3

HCID 81531DiisopropylethylamineHCID 11593468Acetic acid, 2-hydrazinyl-, ethyl ester, hydrochloride (1:1)HCID 866457122-Chloro-N-[(2,2-difluoro-benzo[1,3]dioxol-5-ylamino)-methylsulfanyl-methyl]-6-methyl-isonicotinamide

生成物 1

HCID 59497767[5-(2-Chloro-6-methyl-pyridin-4-yl)-3-(2,2-difluoro-benzo[1,3]dioxol-5-ylamino)-[1,2,4]triazol-1-yl]acetic acid ethyl ester

試薬・触媒・溶媒 1

HCID 6386
tert-Butanol
溶媒

反応条件

温度
60 °C

実験手順

Intermediate D2 (13.6 g; 0.0340 mol), 2-hydrazinylacetic acid ethyl ester, hydrochloride (1:1) (10.5 g; 0.0680 mol), N-ethyl-N-(1-methylethyl)-2-propanamine (13.2 g; 0.1020 mol) and t-BuOH (400 ml) were refluxed for 2 hours. The reaction mixture was then evaporated. Water was added and the product was extracted with CH2Cl2. The organic layer was dried on MgSO4, filtered and evaporated in vacuo. The residue was then heated to 60° C. in ethanol/HCl for 1 hour. The reaction mixture was partly evaporated and, the precipitate was filtered off and dried. Yield: 4.57 g of intermediate D3.

後処理

  1. customThe reaction mixture was then evaporated
  2. additionWater was added
  3. extractionthe product was extracted with CH2Cl2
  4. customThe organic layer was dried on MgSO4
  5. filtrationfiltered
  6. customevaporated in vacuo
  7. customThe reaction mixture was partly evaporated
  8. filtrationthe precipitate was filtered off
  9. customdried

出典と根拠

ORDレコード
ord-19877f1f04394416b80a1aeff2f3b118
出典データセット
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08404851B2

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