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Nicotinic Acid → HCID 15680006、化合物

HRID 703725
ノート
印刷プレビュー

反応式

HRID 703725 の反応式
[C:1]([OH:9])(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[N:4][CH:3]=1.C([N:12]([CH2:15][CH3:16])CC)C.ClC(OCC)=O.N[C:24]1([OH:30])[CH2:29]CC[CH2:26][CH2:25]1>O1CCCC1>[OH:30][CH:24]1[CH2:29][CH2:16][CH:15]([NH:12][C:1]([C:2]2[CH:3]=[N:4][CH:5]=[CH:6][CH:7]=2)=[O:9])[CH2:26][CH2:25]1
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

6

反応物 4

HCID 938Nicotinic AcidHCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 147398371-Aminocyclohexan-1-ol

生成物 1

HCID 15680006HCID 15680006、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
-4 °C

実験手順

Nicotinic acid (2.14 g, 0.017 mol) was suspended in 75 mL of dry tetrahydrofuran, then 1.76 g of freshly distilled triethylamine were added. The clear solution thus obtained was cooled to -4° C. in an ice bath under argon, then ethyl chloroformate (1.88 g, 0.014 mol) in 10 mL of tetrahydrofuran was added such that the temperature did not go above 0° C. The free aminocyclohexanol (2.0 g, 0.017 mol) was added as a powder to the cold reaction mixture, which was allowed to come to room temperature and stirred for 2 hours. The precipitate which formed was collected by filtration, dissolved in 28 mL of hot water and recrystallized as 3.25 g (85%) of fine colorless needles melting at 208°-210° C. and having the formula ##STR112## as confirmed by elemental analysis.

後処理

  1. customThe clear solution thus obtained
  2. customdid not go above 0° C
  3. customto come to room temperature
  4. customThe precipitate which formed
  5. filtrationwas collected by filtration
  6. dissolutiondissolved in 28 mL of hot water
  7. customrecrystallized as 3.25 g (85%) of fine colorless needles melting at 208°-210° C.

出典と根拠

ORDレコード
ord-f6b961da484e4275937a4a70d00245dd
出典データセット
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04983586

反応ノート

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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