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Diisopropylethylamine → 4-[(2-Methoxy-ethyl)-methyl-amino]-but-2-enoic Acid[4-(3-chloro-4-fluoro-phenylamino)-3-cyano-7-methoxy-quinolin-6-yl]-amide Dihydrochloride

HRID 379163
ノート
印刷プレビュー

反応式

HRID 379163 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[O:12][CH3:13])[N:8]=[CH:7][C:6]([C:14]#[N:15])=[C:5]2[NH:16][C:17]1[CH:22]=[CH:21][C:20]([F:23])=[C:19]([Cl:24])[CH:18]=1.C(N(C(C)C)CC)(C)C.Br[CH2:35]/[CH:36]=[CH:37]/[C:38]([Cl:40])=[O:39].[CH3:41][O:42][CH2:43][CH2:44][NH:45][CH3:46].C(=O)(O)[O-].[Na+]>O1CCCC1>[ClH:24].[ClH:40].[Cl:24][C:19]1[CH:18]=[C:17]([NH:16][C:5]2[C:4]3[C:9](=[CH:10][C:11]([O:12][CH3:13])=[C:2]([NH:1][C:38](=[O:39])[CH:37]=[CH:36][CH2:35][N:45]([CH2:44][CH2:43][O:42][CH3:41])[CH3:46])[CH:3]=3)[N:8]=[CH:7][C:6]=2[C:14]#[N:15])[CH:22]=[CH:21][C:20]=1[F:23]
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 5

HCID 81531DiisopropylethylamineHCID 300977(2-Methoxyethyl)(methyl)amineHCID 516892Sodium BicarbonateHCID 111424366-Amino-4-(3-chloro-4-fluoro-phenylamino)-7-methoxy-quinoline-3-carbonitrileHCID 11263885(E)-4-Bromo-2-butenoyl Chloride

生成物 1

HCID 67202828
4-[(2-Methoxy-ethyl)-methyl-amino]-but-2-enoic Acid[4-(3-chloro-4-fluoro-phenylamino)-3-cyano-7-methoxy-quinolin-6-yl]-amide Dihydrochloride

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a stirring solution of 1.2 g (3.5 mmol) of 6-amino-4-(3-chloro-4-fluoro-phenylamino)-7-methoxy-quinoline-3-carbonitrile and 0.52 g (4.0 mmol) of diisopropylethylamine in 40 ml of tetrahydrofuran at 0° C. was added a solution of 4-bromo crotonyl chloride in 10 ml of tetrahydrofuran. After 45 min, 1.87 (21 mmol) of 2-methoxyethyl methyl amine was added. After 1 hr at room temperature, the mixture was poured into a solution of sodium bicarbonate and extracted with ethyl acetate. The organic solution was dried over magnesium sulfate. The solvent was removed and the residue was purified by chromatography on silica gel. Product eluted with ethyl acetate-methanol-triethylamine 40:8:1 giving 0.87 g of the free base. This was dissolved in 20 ml of ethyl acetate and 10 ml of a solution of hydrogen chloride in ether was added. The solid was collected giving 1.02 g of the title compound as a yellow powder: mass spectrum (electrospray, m/e): M+H 498.0, (M+2H)+2248.5.

後処理

  1. waitAfter 1 hr at room temperature
  2. extractionextracted with ethyl acetate
  3. dry with materialThe organic solution was dried over magnesium sulfate
  4. customThe solvent was removed
  5. customthe residue was purified by chromatography on silica gel
  6. washProduct eluted with ethyl acetate-methanol-triethylamine 40:8:1 giving 0.87 g of the free base
  7. dissolutionThis was dissolved in 20 ml of ethyl acetate
  8. addition10 ml of a solution of hydrogen chloride in ether was added
  9. customThe solid was collected

出典と根拠

ORDレコード
ord-85cdb1c000c545b89733c9f41b8611b7
出典データセット
uspto-grants-2001_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06297258B1

反応ノート

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