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Isopropanol → Ammonia methanol

HRID 710211
ノート
印刷プレビュー

反応式

HRID 710211 の反応式
Cl.Cl[C:3]1[N:8]=[C:7]([NH:9][CH:10]2[CH2:15][C:14]([CH3:17])([CH3:16])[NH:13][C:12]([CH3:19])([CH3:18])[CH2:11]2)[C:6]([F:20])=[CH:5][N:4]=1.[CH:21]1([C:24]2[C:29]([N:30]3[CH:34]=[N:33][N:32]=[N:31]3)=[CH:28][C:27]([NH2:35])=[CH:26][C:25]=2[F:36])[CH2:23][CH2:22]1.N1C=NN=N1.C[CH:43]([OH:45])C>>[NH3:4].[CH3:43][OH:45].[CH:21]1([C:24]2[C:29]([N:30]3[CH:34]=[N:33][N:32]=[N:31]3)=[CH:28][C:27]([NH:35][C:3]3[N:8]=[C:7]([NH:9][CH:10]4[CH2:15][C:14]([CH3:17])([CH3:16])[NH:13][C:12]([CH3:19])([CH3:18])[CH2:11]4)[C:6]([F:20])=[CH:5][N:4]=3)=[CH:26][C:25]=2[F:36])[CH2:23][CH2:22]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 3776IsopropanolHCID 58065777HCID 58065777、化合物HCID 86653878HCID 86653878、化合物HCID 178418441HCID 178418441、化合物

生成物 2

HCID 21705897Ammonia methanol収率 1%HCID 56644311HCID 56644311、化合物

反応条件

温度
70 °C

実験手順

A mixture of 2-chloro-5-fluoro-N-(2,2,6,6-tetramethylpiperidin-4-yl)pyrimidin-4-amine hydrochloride (72 mg, 0.190 mmol, 1 equiv), 4-cyclopropyl-3-fluoro-5-(1H-tetrazol-1-yl)benzenamine (50 mg, 0.228 mmol, 1.2 equiv), and PTSA monohydrate (30 mg, 0.152 mmol, 0.8 equiv) in IPA (2 mL) were heated to 70° C. for 3 days. LCMS indicated 2-4% of the cleaved tetrazole product. After cooling to ambient temperature, the crude mixture was quenched with 2M NH3/MeOH followed by concentrating to dryness and repeating once. The crude product was purified by flash chromatography and eluted with DCM:2M NH3/MeOH=100:0 to 96:4 using 1% 2M NH3/MeOH increments to provide the desired product which was recrystallized with IPA/hexane to give desired compound (58 mg, 65%) as a solid.

後処理

  1. temperatureAfter cooling to ambient temperature
  2. customthe crude mixture was quenched with 2M NH3/MeOH
  3. concentrationby concentrating to dryness
  4. customThe crude product was purified by flash chromatography
  5. washeluted with DCM

出典と根拠

ORDレコード
ord-42e54dca3b2c440a817ece6a8759210e
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09181222B2

反応ノート

読み込み中…

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