Water → 2-chloro-N-(1H-indazol-6-yl)-7-tosyl-7H-pyrrolo[2,3-d]pyrimidin-4-amine

HRID 645671

반응식

HRID 645671 반응식
[Cl:1][C:2]1[N:3]=[C:4](Cl)[C:5]2[CH:10]=[CH:9][N:8]([S:11]([C:14]3[CH:20]=[CH:19][C:17]([CH3:18])=[CH:16][CH:15]=3)(=[O:13])=[O:12])[C:6]=2[N:7]=1.[NH2:22][C:23]1[CH:31]=[C:30]2[C:26]([CH:27]=[N:28][NH:29]2)=[CH:25][CH:24]=1.C(N(CC)CC)C.O>C(O)CCC.C(Cl)Cl>[Cl:1][C:2]1[N:3]=[C:4]([NH:22][C:23]2[CH:31]=[C:30]3[C:26]([CH:27]=[N:28][NH:29]3)=[CH:25][CH:24]=2)[C:5]2[CH:10]=[CH:9][N:8]([S:11]([C:14]3[CH:20]=[CH:19][C:17]([CH3:18])=[CH:16][CH:15]=3)(=[O:13])=[O:12])[C:6]=2[N:7]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 814231H-Indazol-6-amineHCID 534868282,4-dichloro-7-tosyl-7H-pyrrolo[2,3-d]pyrimidine

생성물 1

HCID 866280352-chloro-N-(1H-indazol-6-yl)-7-tosyl-7H-pyrrolo[2,3-d]pyrimidin-4-amine수율 95.4%

시약·촉매·용매 2

HCID 2631-Butanol용매HCID 6344Dichloromethane용매

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온도
80 °C

실험 절차

A mixture of 2,4-dichloro-7-tosyl-7H-pyrrolo[2,3-d]pyrimidine (400 mg, 1.17 mmol), 6-aminoindazole (171 mg, 1.29 mmol) and triethylamine (0.400 mL, 2.88 mmol) in n-butyl alcohol (10 mL) was heated at 80° C. overnight. After cooling down, H2O and CH2Cl2 were added. The organic phase was separated, washed with 1N HCl, followed by 5% NaHCO3, before it was dried over Na2SO4 and concentrated in vacuo to give 2-chloro-N-(1H-indazol-6-yl)-7-tosyl-7H-pyrrolo[2,3-d]pyrimidin-4-amine as a solid (490 mg).

후처리

  1. temperatureAfter cooling down
  2. customThe organic phase was separated
  3. washwashed with 1N HCl
  4. dry with materialwas dried over Na2SO4
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-3d71c9c56c3a49abbe358121e17d38b5
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07705004B2

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