Isoamylamine → HCID 57937850, 화합물

HRID 1435082노트

반응식

HRID 1435082 반응식
[CH:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:14]=[CH:13][C:12]([C:15]([NH2:17])=[O:16])=[CH:11][C:10]=2[CH3:18])=[CH:5][CH:4]=1)=O.[CH2:19]([NH2:24])[CH2:20][CH:21]([CH3:23])[CH3:22].[BH4-].[Na+]>CO>[CH3:18][C:10]1[CH:11]=[C:12]([C:15]([NH2:17])=[O:16])[CH:13]=[CH:14][C:9]=1[C:6]1[CH:7]=[CH:8][C:3]([CH2:1][NH:24][CH2:19][CH2:20][CH:21]([CH3:23])[CH3:22])=[CH:4][CH:5]=1

참가 물질

5

반응물 3

HCID 7894IsoamylamineHCID 4311764Sodium borohydrideHCID 57937848HCID 57937848, 화합물

생성물 1

HCID 57937850HCID 57937850, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

4′-Formyl-2-methylbiphenyl-4-carboxamide (I-4a: 4.3 g, 18.0 mmol) and isoamylamine (36.2 mg, 0.425 mmol) were combined in methanol (100 ml). After 12 hours, the reaction mixture was treated with sodium borohydride (2.10 g, 53.9 mmol). After 1 hour, the reaction mixture was treated with concentrated (37%) aqueous hydrochloric acid solution and the volatiles were removed under reduced pressure. The residue was taken up in 2N sodium hydroxide and extracted with ethyl acetate (2 times). The combined organic phases were washed with a saturated aqueous sodium bicarbonate solution, dried over sodium sulfate, filtered and concentrated under reduced pressure to provide the title compound (E4-01).

후처리

  1. waitAfter 1 hour
  2. additionthe reaction mixture was treated
  3. concentrationwith concentrated (37%) aqueous hydrochloric acid solution
  4. customthe volatiles were removed under reduced pressure
  5. extractionextracted with ethyl acetate (2 times)
  6. washThe combined organic phases were washed with a saturated aqueous sodium bicarbonate solution
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-3b91d6089ddf4879903e9f334d88f59a
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07615651B2

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