Hydrazine hydrate (1:1) → HCID 178507266、化合物

HRID 1185106

反応式

HRID 1185106 の反応式
[CH:1]1([C:4](=O)[CH2:5][C:6]#[N:7])[CH2:3][CH2:2]1.O.[NH2:10][NH2:11]>CO>[CH:1]1([C:4]2[CH:5]=[C:6]([NH2:7])[NH:11][N:10]=2)[CH2:3][CH2:2]1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 98127633-Cyclopropyl-3-oxopropanenitrile

生成物 1

HCID 178507266HCID 178507266、化合物収率 46%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
75 °C

実験手順

To a solution of 126a (477 mg, 4.38 mmol) in methanol (5 mL) was added hydrazine hydrate (5 mL, 80%). The reaction mixture was heated at 75° C. for 15 h. The methanol was removed under reduced pressure and the residue was extracted with dichloromethane (2×8 mL). The combined extract was dried over Na2SO4 and concentrated. The residue was purified by flash column eluting with 100:1 dichloromethane/methanol to afford 126b as a yellow oil (250 mg, 46%, over two steps). MS: [M+H]+ 124.

後処理

  1. customThe methanol was removed under reduced pressure
  2. extractionthe residue was extracted with dichloromethane (2×8 mL)
  3. extractionThe combined extract
  4. dry with materialwas dried over Na2SO4
  5. concentrationconcentrated
  6. customThe residue was purified by flash column
  7. washeluting with 100:1 dichloromethane/methanol

出典と根拠

ORDレコード
ord-c09699c258d34e8592ede01c002a7eb1
出典データセット
uspto-grants-2014_03
特許番号
US08669251B2

関連ノート

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