Water → HCID 178525538、化合物

HRID 132465ノート

反応式

HRID 132465 の反応式
[Cl:1][C:2]1[C:10]2[C:9]3[CH2:11][N:12]([CH2:22][C:23]([F:26])([F:25])[F:24])[C:13](=[O:21])[C@H:14]([CH2:16][C:17]([O:19]C)=[O:18])[CH2:15][C:8]=3[CH:7]=[C:6]([Cl:27])[C:5]=2[NH:4][N:3]=1.O.O.[OH-].[Li+]>O1CCCC1.CO>[Cl:1][C:2]1[C:10]2[C:9]3[CH2:11][N:12]([CH2:22][C:23]([F:24])([F:25])[F:26])[C:13](=[O:21])[C@H:14]([CH2:16][C:17]([OH:19])=[O:18])[CH2:15][C:8]=3[CH:7]=[C:6]([Cl:27])[C:5]=2[NH:4][N:3]=1

参加物

6

反応物 3

HCID 962WaterHCID 168937Lithium hydroxide, monohydrateHCID 178500648HCID 178500648、化合物

生成物 1

HCID 178525538HCID 178525538、化合物収率 94%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
50 °C

実験手順

(S)-Methyl 2-(1,4-dichloro-8-oxo-9-(2,2,2-trifluoroethyl)-3,6,7,8,9,10-hexahydroazepino[3,4-e]indazol-7-yl)acetate (230 mg, 0.542 mmol) was dissolved in a mixture of tetrahydrofuran (5.0 mL) and methanol (5.0 mL). Water (5.0 mL) was added to the mixture followed by lithium hydroxide hydrate (66 mg, 1.573 mmol). Reaction was warmed to 50° C. and held with stirring for 4.5 hours. Mixture was cooled to room temperature. Organic solvents were removed from the mixture by roto-vap. Residue was neutralized with 1.6 mL 1N hydrochloric acid. Material was extracted twice with ethyl acetate and the aqueous phase was discarded. Organics were dried MgSO4, filtered and then concentrated to dryness. Title compound was obtained as white solid in 94% yield. MS (M−H)−=407.9, 409.9.

後処理

  1. customReaction
  2. temperatureMixture was cooled to room temperature
  3. customOrganic solvents were removed from the mixture by roto-vap
  4. extractionMaterial was extracted twice with ethyl acetate
  5. filtrationfiltered
  6. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-e27571e615614b4dae2cd2b01c5647bd
出典データセット
uspto-grants-2008_06
特許番号
US07384931B2

反応ノート

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