Ammonium Hydroxide → HCID 178480948、化合物

HRID 51538

反応式

HRID 51538 の反応式
Cl[C:2]1[C:3]2[C:10]([I:11])=[CH:9][N:8]([C@H:12]3[CH2:17][CH2:16][C@H:15]([N:18]4[CH2:23][CH2:22][N:21]([CH3:24])[CH2:20][CH2:19]4)[CH2:14][CH2:13]3)[C:4]=2[N:5]=[CH:6][N:7]=1.[OH-].[NH4+:26]>O1CCOCC1>[I:11][C:10]1[C:3]2[C:2]([NH2:26])=[N:7][CH:6]=[N:5][C:4]=2[N:8]([C@H:12]2[CH2:17][CH2:16][C@H:15]([N:18]3[CH2:23][CH2:22][N:21]([CH3:24])[CH2:20][CH2:19]3)[CH2:14][CH2:13]2)[CH:9]=1

参加物

4

反応物 2

HCID 14923Ammonium HydroxideHCID 178480946HCID 178480946、化合物

生成物 1

HCID 178480948HCID 178480948、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

Trans-4-chloro-5-iodo-7-[4-(4-methylpiperazino)cyclohexyl]-7H-pyrrolo[2,3-d]pyrimidine (0.89 g, 1.9 nmol) in concentrated ammonium hydroxide (40 mL) and dioxane (40 mL) was heated at 120° C. in a pressure vessel for 18 hours. The mixture was allowed to cool to ambient temperature and the solvent was removed under reduced pressure. The residue was partitioned between saturated aqueous sodium bicarbonate solution and ethyl acetate. The water phase was further extracted with ethyl acetate and the combined organic extracts were washed with brine and dried over sodium sulfate. The solvent was removed under reduced pressure to yield trans-5-iodo-7-[4-(4-methylpiperazino)cyclohexyl]-7H-pyrrolo[2,3-d]pyrimidin-4-amine (0.35 g, 0.8 mmol). RP-HPLC (Hypersil C18, 5 μm, 250×4.6 mm; 25%-100% over 15 min with 0.1 M ammnonium acetate, 1 mL/min) Rt 4.01 min. MS: MH+441.

後処理

  1. customthe solvent was removed under reduced pressure
  2. customThe residue was partitioned between saturated aqueous sodium bicarbonate solution and ethyl acetate
  3. extractionThe water phase was further extracted with ethyl acetate
  4. washthe combined organic extracts were washed with brine
  5. dry with materialdried over sodium sulfate
  6. customThe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-aeec641f13a74b2baf49f4c6da0d0a94
出典データセット
uspto-grants-2004_03
特許番号
US06713474B2

関連ノート

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