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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
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Triethylamine → HCID 59758990、化合物

HRID 914391
ノート
印刷プレビュー

反応式

HRID 914391 の反応式
[CH2:1]([NH:8][CH2:9][CH2:10][C:11]1[N:12]=[C:13]([S:16][C:17]([CH3:22])([CH3:21])[C:18]([OH:20])=[O:19])[S:14][CH:15]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH3:7].C(N(CC)CC)C.Cl[C:31]1[C:36]([N+:37]([O-:39])=[O:38])=[CH:35][CH:34]=[CH:33][N:32]=1>C(#N)C>[CH2:1]([N:8]([C:31]1[C:36]([N+:37]([O-:39])=[O:38])=[CH:35][CH:34]=[CH:33][N:32]=1)[CH2:9][CH2:10][C:11]1[N:12]=[C:13]([S:16][C:17]([CH3:21])([CH3:22])[C:18]([OH:20])=[O:19])[S:14][CH:15]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH3:7]
参加物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 8471TriethylamineHCID 796132-Chloro-3-nitropyridineHCID 67399150HCID 67399150、化合物

生成物 1

HCID 59758990HCID 59758990、化合物収率 0.7%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a suspension of 2-({4-[2-(heptylamino)ethyl]-1,3-thiazol-2-yl}thio)-2-methylpropionic acid resin (0.15 g) synthesized in Example 461-6 in acetonitrile (1.5 ml) were added triethylamine (0.16 ml) and 2-chloro-3-nitropyridine (0.089 g), and the mixture was stirred at room temperature overnight. The resin was collected by filtration from the mixture, washed three times with dimethylformamide, tetrahydrofuran and methanol, and vacuum dried. Trifluoroacetic acid (2.0 mL) was added to the obtained resin, and the mixture was left standing at room temperature for 2 hr. Then the resin was removed by filtration from the reaction mixture, and the filtrate was concentrated by blowing a nitrogen gas, vacuum dried, and purified by preparative HPLC to give the title compound (1.5 mg) as a pale-brown oil.

後処理

  1. filtrationThe resin was collected by filtration from the mixture
  2. washwashed three times with dimethylformamide, tetrahydrofuran and methanol, and vacuum
  3. customdried
  4. additionTrifluoroacetic acid (2.0 mL) was added to the obtained resin
  5. waitthe mixture was left
  6. waitstanding at room temperature for 2 hr
  7. customThen the resin was removed by filtration from the reaction mixture
  8. concentrationthe filtrate was concentrated
  9. customdried
  10. custompurified by preparative HPLC

出典と根拠

ORDレコード
ord-243af8cffdef40d487b35152ecd17dc3
出典データセット
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08026370B2

反応ノート

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