Heptane → 2-chloro-3-(1-cyano-1-methylethoxy)-N-{5-[{2-[(cyclopropylcarbonyl)amino][1,3]thiazolo[5,4-b]pyridin-5-yl}(methyl)amino]-2-fluorophenyl}benzamide ethanedioate

HRID 1800641ノート

反応式

HRID 1800641 の反応式
[Cl:1][C:2]1[C:34]([O:35][C:36]([C:39]#[N:40])([CH3:38])[CH3:37])=[CH:33][CH:32]=[CH:31][C:3]=1[C:4]([NH:6][C:7]1[CH:12]=[C:11]([N:13]([C:15]2[N:20]=[C:19]3[S:21][C:22]([NH:24][C:25]([CH:27]4[CH2:29][CH2:28]4)=[O:26])=[N:23][C:18]3=[CH:17][CH:16]=2)[CH3:14])[CH:10]=[CH:9][C:8]=1[F:30])=[O:5].O.O.[C:43]([OH:48])(=[O:47])[C:44]([OH:46])=[O:45].CCCCCCC>C(OCC)(=O)C>[C:43]([OH:48])(=[O:47])[C:44]([OH:46])=[O:45].[Cl:1][C:2]1[C:34]([O:35][C:36]([C:39]#[N:40])([CH3:38])[CH3:37])=[CH:33][CH:32]=[CH:31][C:3]=1[C:4]([NH:6][C:7]1[CH:12]=[C:11]([N:13]([C:15]2[N:20]=[C:19]3[S:21][C:22]([NH:24][C:25]([CH:27]4[CH2:29][CH2:28]4)=[O:26])=[N:23][C:18]3=[CH:17][CH:16]=2)[CH3:14])[CH:10]=[CH:9][C:8]=1[F:30])=[O:5]

参加物

5

反応物 3

HCID 8900HeptaneHCID 61373Oxalic acid dihydrateHCID 252063462-Chloro-3-[(2-Cyanopropan-2-Yl)oxy]-N-{5-[{2-[(Cyclopropylcarbonyl)amino][1,3]thiazolo[5,4-B]pyridin-5-Yl}(Methyl)amino]-2-Fluorophenyl}benzamide

生成物 1

HCID 866460602-chloro-3-(1-cyano-1-methylethoxy)-N-{5-[{2-[(cyclopropylcarbonyl)amino][1,3]thiazolo[5,4-b]pyridin-5-yl}(methyl)amino]-2-fluorophenyl}benzamide ethanedioate収率 98%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

2-Chloro-3-(1-cyano-1-methylethoxy)-N-{5-[{2-[(cyclopropylcarbonyl)amino][1,3]thiazolo[5,4-b]pyridin-5-yl}(methyl)amino]-2-fluorophenyl}benzamide (300 mg, 0.518 mmol) produced in Example C122(xi) was dissolved in ethyl acetate (9 mL), oxalic acid dihydrate (68.6 mg, 0.544 mmol) was added, and the mixture was stood at 55° C. To the obtained solution was added heptane, and the mixture was cooled to room temperature. The crystallized crystals were collected by filtration, and dried to give the title compound (339 mg, 98%) as colorless crystals.

後処理

  1. customwas stood at 55° C
  2. filtrationThe crystallized crystals were collected by filtration
  3. customdried

出典と根拠

ORDレコード
ord-1ffbec1a67be4f6da5eabc410aa509eb
出典データセット
uspto-grants-2013_01
特許番号
US08344135B2

反応ノート

読み込み中…