Hydrochloric Acid → Dodecane-1-sulfonic acid [5-(5,6-difluoro-1H-indol-2-yl)-methoxy-phenyl]-amide

HRID 25508

反応式

HRID 25508 の反応式
[CH2:1]([S:13](Cl)(=[O:15])=[O:14])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].[F:17][C:18]1[CH:19]=[C:20]2[C:24](=[CH:25][C:26]=1[F:27])[NH:23][C:22]([C:28]1[CH:29]=[CH:30][C:31]([O:35][CH3:36])=[C:32]([NH2:34])[CH:33]=1)=[CH:21]2.O.Cl>N1C=CC=CC=1>[F:17][C:18]1[CH:19]=[C:20]2[C:24](=[CH:25][C:26]=1[F:27])[NH:23][C:22]([C:28]1[CH:29]=[CH:30][C:31]([O:35][CH3:36])=[C:32]([NH:34][S:13]([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12])(=[O:15])=[O:14])[CH:33]=1)=[CH:21]2

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 66280Dodecylsulfonyl chlorideHCID 99434395-(5,6-difluoro1H-indol-2-yl)-2-methoxy-phenylamine

生成物 1

HCID 10300955Dodecane-1-sulfonic acid [5-(5,6-difluoro-1H-indol-2-yl)-methoxy-phenyl]-amide収率 44.9%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

1-Dodecanesulfonyl chloride (0.3 g, 1.1 mmol) was added to a stirred solution of 5-(5,6-difluoro-1H-indol-2-yl)-2-methoxy-phenyl-amine from Example 3 (0.3 g, 1.11 mmol) in pyridine (3 mL) under an inert atmosphere at room temperature. After approximately 20 hours the mixture was poured into water (30 mL), stirred, and acidified with aqueous HCl. After several hours the precipitate was filtered off, rinsed three times with water, and dried. Recrystallization from ethanol afforded the product (0.25 g), mp 148-149° C.

後処理

  1. filtrationAfter several hours the precipitate was filtered off
  2. washrinsed three times with water
  3. customdried
  4. customRecrystallization from ethanol

出典と根拠

ORDレコード
ord-d578a370dc0942399ec5b135fdf01bfd
出典データセット
uspto-grants-2005_02
特許番号
US06858739B2

関連ノート

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