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Hydrochloric Acid → HCID 69179467、化合物

HRID 1071936
ノート
印刷プレビュー

反応式

HRID 1071936 の反応式
Cl[C:2]1[N:7]=[C:6]([NH:8][CH2:9][CH2:10][CH2:11][N:12]2[CH2:17][CH2:16][O:15][CH2:14][CH2:13]2)[C:5]([C:18]#[N:19])=[CH:4][N:3]=1.[O:20]1[CH2:24][CH2:23][CH2:22][CH:21]1[CH2:25][NH:26][S:27]([C:30]1[CH:36]=[CH:35][C:33]([NH2:34])=[CH:32][CH:31]=1)(=[O:29])=[O:28].Cl>CC(O)CC>[C:18]([C:5]1[C:6]([NH:8][CH2:9][CH2:10][CH2:11][N:12]2[CH2:17][CH2:16][O:15][CH2:14][CH2:13]2)=[N:7][C:2]([NH:34][C:33]2[CH:32]=[CH:31][C:30]([S:27](=[O:29])(=[O:28])[NH:26][CH2:25][CH:21]3[CH2:22][CH2:23][CH2:24][O:20]3)=[CH:36][CH:35]=2)=[N:3][CH:4]=1)#[N:19]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 47135324-amino-N-(tetrahydrofuran-2-ylmethyl)benzenesulfonamideHCID 22390639HCID 22390639、化合物

生成物 1

HCID 69179467HCID 69179467、化合物収率 13.2%

試薬・触媒・溶媒 1

HCID 6568(+-)-2-Butanol溶媒

実験手順

2Chloro-5-cyano-4-(3-morpholinopropylamino)pyrimidine (Method 66; 525 mg, 1.87 mmol), 4-[N-(tetrahydrofur-2-ylmethyl)sulphamoyl]aniline (Method 2; 430 mg, 1.68 mmol) and 1M ethereal hydrogen chloride (1.87 ml, 1.87 mmol) in 2-butanol (3 ml) was heated at 90° C. for 3 hours. The mixture was allowed to cool, the resulting precipitate was collected by filtration and was washed with ethyl acetate. The crude solid was purified by chromatography eluting with DCM/methanolic ammonia/(100:0) increasing in polarity to (97:3). The product was recrystallized from methanol to give the title compound (111 mg).

後処理

  1. temperatureto cool
  2. filtrationthe resulting precipitate was collected by filtration
  3. washwas washed with ethyl acetate
  4. customThe crude solid was purified by chromatography
  5. washeluting with DCM/methanolic ammonia/(100:0)
  6. temperatureincreasing in polarity to (97:3)
  7. customThe product was recrystallized from methanol

出典と根拠

ORDレコード
ord-a8b1071404cb491880e3613f7649aba1
出典データセット
uspto-grants-2005_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06908920B2

反応ノート

読み込み中…

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