5-Methylindoline → HCID 20231382、化合物

HRID 717782

反応式

HRID 717782 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[NH:7][CH2:6][CH2:5]2.[N:11]([O-])=[O:12].[Na+]>Cl.O>[CH3:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[N:7]([N:11]=[O:12])[CH2:6][CH2:5]2

参加物

5

反応物 2

HCID 140236795-MethylindolineHCID 23668193Sodium Nitrite

生成物 1

HCID 20231382HCID 20231382、化合物収率 98.7%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

5-Methylindoline (1.0 g, 7.5 mmol) was stirred in 3N HCl (20 mL) at 0° C. Sodium nitrite (0.621 g, 9.0 mmol) in water (2 mL) was added dropwise and the mixture was stirred at 0° C. for 5 min. followed by RT for 20 min. The reaction mixture was extracted with DCM (500 mL), and the organic layer was dried over sodium sulfate and concentrated under vacuum to obtain 1.2 g of 5-methyl-1-nitrosoindoline.

後処理

  1. waitfollowed by RT for 20 min
  2. extractionThe reaction mixture was extracted with DCM (500 mL)
  3. dry with materialthe organic layer was dried over sodium sulfate
  4. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-87962a4fe92a449ba21dd06f782d09e1
出典データセット
uspto-grants-2015_11
特許番号
US09193728B2

関連ノート

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