Butylamine → 85262-77-7

HRID 615629노트

반응식

HRID 615629 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:9]=[C:10]([Cl:12])[CH:11]=1)[O:5][CH2:6][CH2:7]Br.[CH2:13]([NH2:17])[CH2:14][CH2:15][CH3:16]>>[ClH:1].[Cl:1][C:2]1[CH:3]=[C:4]([CH:9]=[C:10]([Cl:12])[CH:11]=1)[O:5][CH2:6][CH2:7][NH:17][CH2:13][CH2:14][CH2:15][CH3:16]

참가 물질

3

반응물 2

HCID 8007ButylamineHCID 222467761-(2-Bromoethoxy)-3,5-dichlorobenzene

생성물 1

HCID 2025633585262-77-7수율 51.5%

실험 절차

A solution of 33.76 g (0.126 mole) of 2-(3,5-dichlorophenoxy)-1-bromoethane in 200 ml of n-butylamine was stirred at 25° C. for 20 hr. The excess n-butylamine was evaporated in vacuo, and the residue was suspended in a mixture of dilute sodium hydroxide and shaken with methylene chloride. The methylene chloride layer was extracted in sequence with two additional portions of dilute sodium hydroxide, one of dilute sulfuric acid and once more with dilute sodium hydroxide. The volume of the methylene chloride layer was reduced to about 150 ml and excess ethereal hydrogen chloride was added. Addition of anhydrous ether gave a white precipitate which was collected and dried under high vacuum (78° C.) to give 19.35 g (51.5%) white crystals, m.p. 195°-196° C.

후처리

  1. customThe excess n-butylamine was evaporated in vacuo
  2. additionthe residue was suspended in a mixture of dilute sodium hydroxide
  3. extractionThe methylene chloride layer was extracted in sequence with two additional portions of dilute sodium hydroxide, one of dilute sulfuric acid and once more with dilute sodium hydroxide
  4. additionwas added
  5. additionAddition of anhydrous ether
  6. customgave a white precipitate which
  7. customwas collected
  8. customdried under high vacuum (78° C.)

출처 및 근거

ORD 기록
ord-2ca0e35461fc4ee8a73f71c94d2bc1da
출처 데이터셋
uspto-grants-1985_02
특허 번호
US04500529

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