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Hydrochloric Acid → 2-[(3S,4R)-4-{[(3,4-dichloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}-3-methoxypiperidin-1-yl]-4-{5-[2-(pyrrolidin-1-yl)ethoxy]pyrazin-2-yl}-1,3-thiazole-5-carboxylic acid

HRID 655737
ノート
印刷プレビュー

反応式

HRID 655737 の反応式
[N:1]1([CH2:6][CH2:7][OH:8])[CH2:5][CH2:4][CH2:3][CH2:2]1.[H-].[Na+].Cl[C:12]1[N:13]=[CH:14][C:15]([C:18]2[N:19]=[C:20]([N:28]3[CH2:33][CH2:32][C@H:31]([NH:34][C:35]([C:37]4[NH:38][C:39]([CH3:44])=[C:40]([Cl:43])[C:41]=4[Cl:42])=[O:36])[C@H:30]([O:45][CH3:46])[CH2:29]3)[S:21][C:22]=2[C:23]([O:25]CC)=[O:24])=[N:16][CH:17]=1.Cl>O1CCCC1.C(#N)C>[Cl:42][C:41]1[C:40]([Cl:43])=[C:39]([CH3:44])[NH:38][C:37]=1[C:35]([NH:34][C@@H:31]1[CH2:32][CH2:33][N:28]([C:20]2[S:21][C:22]([C:23]([OH:25])=[O:24])=[C:18]([C:15]3[CH:14]=[N:13][C:12]([O:8][CH2:7][CH2:6][N:1]4[CH2:5][CH2:4][CH2:3][CH2:2]4)=[CH:17][N:16]=3)[N:19]=2)[CH2:29][C@@H:30]1[O:45][CH3:46])=[O:36]
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

7

反応物 4

HCID 313Hydrochloric AcidHCID 24758Sodium hydrideHCID 762881-PyrrolidineethanolHCID 59402528ethyl 4-(5-chloropyrazin-2-yl)-2-[(3R,4S)-4-{[(3,4-dichloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}-3-methoxypiperidin-1-yl]-1,3-thiazole-5-carboxylate

生成物 1

HCID 58075010
2-[(3S,4R)-4-{[(3,4-dichloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}-3-methoxypiperidin-1-yl]-4-{5-[2-(pyrrolidin-1-yl)ethoxy]pyrazin-2-yl}-1,3-thiazole-5-carboxylic acid
収率 45%

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
80 °C

実験手順

To a stirred solution of 2-(pyrrolidine-1-yl)ethanol (0.102 mL, 0.872 mmol) in dry tetrahydrofuran (20 mL) was added sodium hydride (70 mg, 1.771 mmol) at 0° C. The reaction mixture was heated to 80° C. After 10 min, ethyl 4-(5-chloropyrazin-2-yl)-2-[(3S,4R)-4-{[(3,4-dichloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}-3-methoxypiperidin-1-yl]-1,3-thiazole-5-carboxylate (Example 59, 250 mg, 0.436 mmol) was added to the reaction mixture at 80° C. and further maintained at 80° C. for 10 min. After the completion of the reaction, the reaction mixture was cooled and carefully quenched by adding ice pieces. The aqueous layer was extracted with ethyl acetate (2×50 mL) to get rid of any organic impurities and discarded. The aqueous layer was acidified to pH=2 using 2N HCl solution and was extracted with 10% methanol/dichloromethane (2×100 mL). The organic layer was dried and concentrated under reduced pressure to yield the product. The obtained product was stirred in acetonitrile (10 mL). The solid was filtered and dried to obtain 120 mg (45%) of 2-[(3S,4R)-4-{[(3,4-dichloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}-3-methoxypiperidin-1-yl]-4-{5-[2-(pyrrolidin-1-yl)ethoxy]pyrazin-2-yl}-1,3-thiazole-5-carboxylic acid as yellow solid.

後処理

  1. temperaturefurther maintained at 80° C. for 10 min
  2. customAfter the completion of the reaction
  3. temperaturethe reaction mixture was cooled
  4. customcarefully quenched
  5. additionby adding ice pieces
  6. extractionThe aqueous layer was extracted with ethyl acetate (2×50 mL)
  7. customto get rid of any organic impurities
  8. extractionwas extracted with 10% methanol/dichloromethane (2×100 mL)
  9. customThe organic layer was dried
  10. concentrationconcentrated under reduced pressure
  11. customto yield the product
  12. filtrationThe solid was filtered
  13. customdried

出典と根拠

ORDレコード
ord-9f35500346a7401a8bc81fea57cc3773
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08071605B2

反応ノート

読み込み中…

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