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Hydrochloric Acid → HCID 15615501、化合物

HRID 1194312
ノート
印刷プレビュー

反応式

HRID 1194312 の反応式
[CH:1]([NH:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)=O.[Cl:10][C:11]1[CH:16]=[C:15]([O:17][CH3:18])[N:14]=C(S(C)(=O)=O)[N:12]=1.Cl>O1CCCC1.O>[NH:3]([C:1]1[N:12]=[C:11]([Cl:10])[CH:16]=[C:15]([O:17][CH3:18])[N:14]=1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 7671FormanilideHCID 137292254-Chloro-2-(methanesulfonyl)-6-methoxypyrimidine

生成物 1

HCID 15615501HCID 15615501、化合物収率 114.5%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

1.8 g of formanilide was dissolved in 50 ml of tetrahydrofuran, and 0.4 g of sodium hydride from which the oily matter had been removed before hand with n-hexane was slowly added to the resulting solution at 10° to 20° C. while cooling with ice water. To the suspension thus obtained was added 3.3 g of 4-chloro-2-methanesulfonyl-6-methoxypyrimidine, and the mixture was stirred for 1 hour at room temperature. Then, 15 ml of 4N hydrochloric acid was added, and reaction was effected for 1 hour under reflux. The reaction liquid was poured in water, extracted with ether, and the ether layer was washed with water, dried over magnesium sulfate, and then the ether was stripped by concentration. The residual crystals were recrystallized from n-hexane, and 4.0 g of 2-anilino-4-chloro-6-methoxypyrimidine was obtained (yield 87%). Melting point: 101°-103° C.

後処理

  1. custom0.4 g of sodium hydride from which the oily matter had been removed before hand with n-hexane
  2. additionwas slowly added to the resulting solution at 10° to 20° C.
  3. temperaturewhile cooling with ice water
  4. customTo the suspension thus obtained
  5. customreaction
  6. waitwas effected for 1 hour
  7. temperatureunder reflux
  8. customThe reaction liquid
  9. extractionextracted with ether
  10. washthe ether layer was washed with water
  11. dry with materialdried over magnesium sulfate
  12. concentrationthe ether was stripped by concentration
  13. customThe residual crystals were recrystallized from n-hexane

出典と根拠

ORDレコード
ord-980d832fa79b4bb79e3ceb9b3eb2e60c
出典データセット
uspto-grants-1989_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04814338

反応ノート

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