Water → Tak-137

HRID 1405869ノート

反応式

HRID 1405869 の反応式
[O:1]([C:8]1[CH:13]=[CH:12][C:11]([C:14]2[C:15]([NH2:20])=[N:16][CH:17]=[CH:18][CH:19]=2)=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl[CH2:22][CH2:23][S:24](Cl)(=[O:26])=[O:25].O>CN(C)C(=O)C>[O:1]([C:8]1[CH:13]=[CH:12][C:11]([C:14]2[C:15]3=[N:20][S:24](=[O:26])(=[O:25])[CH2:23][CH2:22][N:16]3[CH:17]=[CH:18][CH:19]=2)=[CH:10][CH:9]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 962WaterHCID 15385Ethanesulfonylchloride, 2-chloro-HCID 655512093-(4-Phenoxyphenyl)pyridin-2-amine

生成物 1

HCID 56649286Tak-137収率 85.7%

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒2 回

反応条件

温度
60 °C

実験手順

A solution of 3-(4-phenoxyphenyl)pyridin-2-amine (301 mg) in N,N-dimethylacetoamide (3 mL) was added dropwise to 2-chloroethanesulfonyl chloride (382 mg) and additional N,N-dimethylacetoamide (2 mL) was used to complete the addition of above solution. After being stirred at 60° C. for 4 hr, the mixture was cooled to room temperature. Water (10 mL) was added dropwise to the reaction mixture and the whole was stirred at room temperature for 0.5 hr. The precipitate was collected by filtration, washed with water (10 mL) and THF (3 mL), and dried in vacuo at 60° C. to give the title compound (346.7 mg) as an off-white powder.

後処理

  1. additionthe addition of above solution
  2. temperaturethe mixture was cooled to room temperature
  3. stirringthe whole was stirred at room temperature for 0.5 hr
  4. filtrationThe precipitate was collected by filtration
  5. washwashed with water (10 mL) and THF (3 mL)
  6. customdried in vacuo at 60° C.

出典と根拠

ORDレコード
ord-efa28ae00b3c4eb98d1cf79a00dafcf5
出典データセット
uspto-grants-2014_12
特許番号
US08916551B2

反応ノート

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