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Hydrochloric Acid → HCID 57520170、化合物

HRID 1528101
ノート
印刷プレビュー

反応式

HRID 1528101 の反応式
[NH:1]1[CH2:6][CH:5]=[C:4]([C:7]2[CH:8]=[C:9]3[C:14](=[CH:15][CH:16]=2)[N:13]=[CH:12][CH:11]=[C:10]3[NH:17][C:18]([NH:20][C:21]2[CH:26]=[CH:25][CH:24]=[C:23]([C:27]([F:30])([F:29])[F:28])[N:22]=2)=[O:19])[CH2:3][CH2:2]1.[CH2:31]=O.[BH4-].[Na+].Cl>O.CO>[CH3:31][N:1]1[CH2:2][CH:3]=[C:4]([C:7]2[CH:8]=[C:9]3[C:14](=[CH:15][CH:16]=2)[N:13]=[CH:12][CH:11]=[C:10]3[NH:17][C:18]([NH:20][C:21]2[CH:26]=[CH:25][CH:24]=[C:23]([C:27]([F:29])([F:30])[F:28])[N:22]=2)=[O:19])[CH2:5][CH2:6]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 4311764Sodium borohydrideHCID 57520094HCID 57520094、化合物

生成物 1

HCID 57520170HCID 57520170、化合物収率 96.8%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒
HCID 962
Water
溶媒

実験手順

To 0.12 g of 1-[6-(1,2,3,6-tetrahydro-pyridin-4-yl)-quinolin-4-yl]-3-(6-trifluoromethyl-pyridin-2-yl)-urea (0.290 mmol) were added subsequently 2 ml of methanol, 0.366 ml of formaldehyde (4.64 mmol) and a solution of 0.055 g of sodium borohydride (1.451 mmol) in 0.8 ml of water. The reaction was slightly exotherm. A small amount of 2M HCl was added to the reaction mixture up to a pH of 3 to destroy the excess of sodium bororhydride. After neutralization with sodium bicarbonate, methanol was evaporated under reduced pressure, water added to the residue, the reaction mixture extracted three times with ethylacetate, the organic phases combined and dried over sodium sulfate and the solvent evaporated under reduced pressure. 120 mg of the desired product were obtained as an off white powder (yield: 97%).

後処理

  1. customto destroy the excess of sodium bororhydride
  2. customAfter neutralization with sodium bicarbonate, methanol was evaporated under reduced pressure, water
  3. additionadded to the residue
  4. extractionthe reaction mixture extracted three times with ethylacetate
  5. dry with materialdried over sodium sulfate
  6. customthe solvent evaporated under reduced pressure

出典と根拠

ORDレコード
ord-e194a1a72db2400a91363918be88c240
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09090592B2

反応ノート

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