Hydrazine hydrate (1:1) → HCID 178507266, 화합물

HRID 1185106

반응식

HRID 1185106 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 178507266HCID 178507266, 화합물수율 46%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
75 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c09699c258d34e8592ede01c002a7eb1
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08669251B2

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