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Hydrochloric Acid → 2-[2-[(4aR,7aR)-2-Amino-7a-isothiazol-5-yl-4,4a,5,7-tetrahydropyrrolo[3,4-d][1,3]thiazin-6-yl]-5-fluoro-6-methyl-pyrimidin-4-yl]propan-2-ol hydrochloride

HRID 1619075
ノート
印刷プレビュー

反応式

HRID 1619075 の反応式
[F:1][C:2]1[C:3]([C:32]([OH:35])([CH3:34])[CH3:33])=[N:4][C:5]([N:9]2[CH2:17][C@@H:16]3[C@@:11]([C:27]4[S:31][N:30]=[CH:29][CH:28]=4)([N:12]=[C:13]([NH:18]C(=O)C4C=CC=CC=4)[S:14][CH2:15]3)[CH2:10]2)=[N:6][C:7]=1[CH3:8].N1C=CC=CC=1.[ClH:42].CON.Cl.O1CCOCC1>C(O)C.C(Cl)Cl>[ClH:42].[NH2:18][C:13]1[S:14][CH2:15][C@@H:16]2[CH2:17][N:9]([C:5]3[N:4]=[C:3]([C:32]([OH:35])([CH3:34])[CH3:33])[C:2]([F:1])=[C:7]([CH3:8])[N:6]=3)[CH2:10][C@:11]2([C:27]2[S:31][N:30]=[CH:29][CH:28]=2)[N:12]=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

8

反応物 5

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 312751,4-DioxaneHCID 521874O-Methylhydroxylamine hydrochlorideHCID 86762241N-[(4aR,7aR)-6-[5-Fluoro-4-(1-hydroxy-1-methyl-ethyl)-6-methyl-pyrimidin-2-yl]-7a-isothiazol-5-yl-4,4a,5,7-tetrahydropyrrolo[3,4-d][1,3]thiazin-2-yl]benzamide

生成物 1

HCID 86762256
2-[2-[(4aR,7aR)-2-Amino-7a-isothiazol-5-yl-4,4a,5,7-tetrahydropyrrolo[3,4-d][1,3]thiazin-6-yl]-5-fluoro-6-methyl-pyrimidin-4-yl]propan-2-ol hydrochloride
収率 62.5%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
70 °C

実験手順

N-[(4aR,7aR)-6-[5-Fluoro-4-(1-hydroxy-1-methyl-ethyl)-6-methyl-pyrimidin-2-yl]-7a-isothiazol-5-yl-4,4a,5,7-tetrahydropyrrolo[3,4-d][1,3]thiazin-2-yl]benzamide (33 mg, 0.064 mmol) is dissolved in ethanol (2 mL). To this solution is added pyridine (0.052 mL, 0.6 mmol) and O-methylhydroxylamine hydrochloride (55 mg, 0.6 mmol). The reaction is warmed to 70° C. for 4 hours. The reaction is cooled to room temperature and stirred overnight (˜16 hrs). The mixture is concentrated to give the crude product which is purified via silica gel chromatography using a 0-10% (7 N NH3 in MeOH)/DCM to give the pure freebase. The freebase is dissolved in DCM (2 mL) and treated with 4 M HCl in dioxane (0.3 mL, 1.2 mmol). The mixture is concentrated to give the title compound as a white solid (18 mg, 0.04 mmol). ES/MS (m/z): 409 (M+H). [α]D20=−6.0° (C=1.0, MeOH).

後処理

  1. temperatureThe reaction is cooled to room temperature
  2. concentrationThe mixture is concentrated
  3. customto give the crude product which
  4. customis purified via silica gel chromatography
  5. customto give the pure freebase
  6. concentrationThe mixture is concentrated

出典と根拠

ORDレコード
ord-b35781ca70784f65b8137e90c3a7956a
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08772282B2

反応ノート

読み込み中…

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