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

Triethylamine → Tris(1,1-dimethylethyl) 2-{2-chloro-5-fluoro-6-[(1,3-thiazol-4-ylmethyl)amino]-4-pyrimidinyl}-1,1,2-hydrazinetricarboxylate

HRID 1366672
ノート
印刷プレビュー

反応式

HRID 1366672 の反応式
[S:1]1[CH:5]=[C:4]([CH2:6][NH2:7])[N:3]=[CH:2]1.[CH3:8][C:9]([O:12][C:13]([N:15]([C:33]([O:35][C:36]([CH3:39])([CH3:38])[CH3:37])=[O:34])[N:16]([C:24]1[C:29]([F:30])=[C:28](Cl)[N:27]=[C:26]([Cl:32])[N:25]=1)[C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])=[O:14])([CH3:11])[CH3:10].C(N(CC)CC)C>C1COCC1.O>[CH3:11][C:9]([O:12][C:13]([N:15]([C:33]([O:35][C:36]([CH3:39])([CH3:38])[CH3:37])=[O:34])[N:16]([C:24]1[C:29]([F:30])=[C:28]([NH:7][CH2:6][C:4]2[N:3]=[CH:2][S:1][CH:5]=2)[N:27]=[C:26]([Cl:32])[N:25]=1)[C:17]([O:19][C:20]([CH3:21])([CH3:22])[CH3:23])=[O:18])=[O:14])([CH3:8])[CH3:10]
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 3

HCID 8471TriethylamineHCID 150636521,3-Thiazol-4-ylmethanamineHCID 58000755Tris(1,1-dimethylethyl) 2-(2,6-dichloro-5-fluoro-4-pyrimidinyl)-1,1,2-hydrazinetricarboxylate

生成物 1

HCID 86637026Tris(1,1-dimethylethyl) 2-{2-chloro-5-fluoro-6-[(1,3-thiazol-4-ylmethyl)amino]-4-pyrimidinyl}-1,1,2-hydrazinetricarboxylate収率 68%

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 8028Tetrahydrofuran溶媒3 回

実験手順

To a suspension of (1,3-thiazol-4-ylmethyl)amine (0.1491 g, 1.308 mmol) in THF (10 mL) was added a solution of tris(1,1-dimethylethyl)2-(2,6-dichloro-5-fluoro-4-pyrimidinyl)-1,1,2-hydrazinetricarboxylate (0.649 g, 1.308 mmol) and triethylamine (0.22 mL, 1.5784 mmol) in THF (2 mL). Additional THF (3 mL) was added, and the reaction was stirred overnight. Then the reaction mixture was diluted with water, and the aqueous layer was extracted with ethyl acetate. The organics were dried (Na2SO4) and concentrated. The resulting crude material was purified by silica gel chromatography (0-100% ethyl acetate in hexanes) to produce tris(1,1-dimethylethyl)2-{2-chloro-5-fluoro-6-[(1,3-thiazol-4-ylmethyl)amino]-4-pyrimidinyl}-1,1,2-hydrazinetricarboxylate as a yellow oil (0.51 g, 68%). LCMS: (M-2Boc)=375.0.

後処理

  1. extractionthe aqueous layer was extracted with ethyl acetate
  2. dry with materialThe organics were dried (Na2SO4)
  3. concentrationconcentrated
  4. customThe resulting crude material was purified by silica gel chromatography (0-100% ethyl acetate in hexanes)

出典と根拠

ORDレコード
ord-5d8d4b4ffacf474db23e61dc851c9a93
出典データセット
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07893056B2

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