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Hydrochloric Acid → HCID 178483082、化合物

HRID 1984875
ノート
印刷プレビュー

反応式

HRID 1984875 の反応式
C(OC(=O)[NH:7][CH2:8][C@H:9]1[CH2:14][CH2:13][C@H:12]([NH:15][C:16]2[N:25]=[C:24]([N:26]([CH3:28])[CH3:27])[C:23]3[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=3)[N:17]=2)[CH2:11][CH2:10]1)(C)(C)C.Cl.C(N(C(C)C)CC)(C)C.[Br:40][C:41]1[CH:46]=[CH:45][C:44]([S:47](Cl)(=[O:49])=[O:48])=[C:43]([O:51][C:52]([F:55])([F:54])[F:53])[CH:42]=1>CCOC(C)=O.C(Cl)Cl>[Br:40][C:41]1[CH:46]=[CH:45][C:44]([S:47]([NH:7][CH2:8][C@H:9]2[CH2:10][CH2:11][C@H:12]([NH:15][C:16]3[N:25]=[C:24]([N:26]([CH3:28])[CH3:27])[C:23]4[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=4)[N:17]=3)[CH2:13][CH2:14]2)(=[O:49])=[O:48])=[C:43]([O:51][C:52]([F:55])([F:54])[F:53])[CH:42]=1
参加物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 81531Diisopropylethylamine2 回HCID 27364214-Bromo-2-(Trifluoromethoxy)Benzene-1-Sulfonyl Chloride2 回HCID 178483080HCID 178483080、化合物

生成物 1

HCID 178483082HCID 178483082、化合物収率 83%

試薬・触媒・溶媒 2

HCID 6344
Dichloromethane
溶媒
3 回
HCID 8857Ethyl Acetate溶媒2 回

実験手順

To a suspension of trans-[4-(4-dimethylamino-quinazolin-2-ylamino)-cyclohexylmethyl]-carbamic acid tert-butyl ester (500 mg, 1.25 mmol) in EtOAc (5 mL) was added 4 M hydrogen chloride in EtOAc (5 mL). The mixture was stirred at ambient temperature for 1 hr and concentrated to give a white solid. To a suspension of the above solid in CH2Cl2 (7 mL) was added diisopropylethylamine (905 μL, 5.20 mmol). The mixture was cooled to 4° C. and a solution of 4-bromo-2-trifluoromethoxy-benzenesulfonyl chloride (446 mg, 1.31 mmol) in CH2Cl2 (2 mL) was added below 5° C. The reaction mixture was stirred at 4° C. for 1.5 hr. To the reaction mixture was added a solution of 4-bromo-2-trifluoromethoxy-benzenesulfonyl chloride (85 mg, 0.25 mmol) in CH2Cl2 (0.5 mL) and the mixture was stirred at 4° C. for 1 hr. To the reaction mixture was added diisopropylethylamine (220 μL, 1.26 mmol) and the mixture was stirred at 4° C. for 1 hr. The reaction was quenched with saturated aqueous NaHCO3. The aqueous layer was extracted with CHCl3 (three times). The combined organic layer was dried over MgSO4, filtered, concentrated, and purified by flash chromatography (NH-silica gel, 50% EtOAc in hexane) to give trans-4-bromo-N-[4-(4-dimethylamino-quinazolin-2-ylamino)-cyclohexylmethyl]-2-trifluoromethoxy-benzenesulfonamide (624 mg, 83%) as a pale yellow solid.

後処理

  1. concentrationconcentrated
  2. customto give a white solid
  3. temperatureThe mixture was cooled to 4° C.
  4. stirringThe reaction mixture was stirred at 4° C. for 1.5 hr
  5. stirringthe mixture was stirred at 4° C. for 1 hr
  6. stirringthe mixture was stirred at 4° C. for 1 hr
  7. customThe reaction was quenched with saturated aqueous NaHCO3
  8. extractionThe aqueous layer was extracted with CHCl3 (three times)
  9. dry with materialThe combined organic layer was dried over MgSO4
  10. filtrationfiltered
  11. concentrationconcentrated
  12. custompurified by flash chromatography (NH-silica gel, 50% EtOAc in hexane)

出典と根拠

ORDレコード
ord-72b5fcdd57c14018b555336494b668f7
出典データセット
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07544690B2

反応ノート

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