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Water → 2-(Quinolin-4-ylmethylthio)pyridine-3-carboxylic acid

HRID 599360
ノート
印刷プレビュー

反応式

HRID 599360 の反応式
C(N(CC)CC)C.Cl[CH2:9][C:10]1[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[N:13]=[CH:12][CH:11]=1.[SH:20][C:21]1[N:29]=[CH:28][CH:27]=[CH:26][C:22]=1[C:23]([OH:25])=[O:24].O>CN(C)C=O.C(OCC)(=O)C>[N:13]1[C:14]2[C:19](=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:10]([CH2:9][S:20][C:21]2[C:22]([C:23]([OH:25])=[O:24])=[CH:26][CH:27]=[CH:28][N:29]=2)=[CH:11][CH:12]=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 962WaterHCID 8471TriethylamineHCID 123557014-(Chloromethyl)quinolineHCID 178524460HCID 178524460、化合物

生成物 1

HCID 670539532-(Quinolin-4-ylmethylthio)pyridine-3-carboxylic acid収率 59%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒
HCID 8857
Ethyl Acetate
溶媒

実験手順

Triethylamine (33 mL, 240 mmol) was added to a suspension of a mixture containing 4-(chloromethyl) quinoline (Reference Compound No. 5-1, 17.0 g) and 2-mercaptonicotinic acid (13 g, 86 mmol) in anhydrous N,N-dimethylformamide (200 mL) at room temperature, and the mixture was stirred for 48 hours. Water (700 mL) and ethyl acetate (400 mL) were added thereto. After the mixture was separated into the organic layer and the aqueous layer, 1N hydrochloric acid (50 mL) was added to the aqueous layer. The precipitated solid was filtered off and dried under reduced pressure at 60° C. to give 15 g of the title Reference Compound as a yellow solid (Yield: 59%).

後処理

  1. customAfter the mixture was separated into the organic layer
  2. additionthe aqueous layer, 1N hydrochloric acid (50 mL) was added to the aqueous layer
  3. filtrationThe precipitated solid was filtered off
  4. customdried under reduced pressure at 60° C.

出典と根拠

ORDレコード
ord-457d7a41ab08491f858562b5f7087a3e
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07897774B2

反応ノート

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