Hydrochloric Acid → tert-Butyl propiolate

HRID 14282

반응식

HRID 14282 반응식
[C:1]([O:5][C:6](=[O:33])NC(CC1C=C(F)C=C(F)C=1)C(O)CNC1(C2C=CC=C(C#C)C=2)CC1)([CH3:4])([CH3:3])[CH3:2].Cl.CO.O1CCO[CH2:39][CH2:38]1>>[C:6]([C:38]#[CH:39])([O:5][C:1]([CH3:2])([CH3:3])[CH3:4])=[O:33]

참가 물질

5

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 312751,4-DioxaneHCID 21062898[1-(3,5-Difluorobenzyl)-3-[1-(3-ethynylphenyl)cyclopropylamino]-2-hydroxypropyl]-carbamic acid tert-butyl ester

생성물 1

HCID 543038tert-Butyl propiolate수율 106%

실험 절차

[1-(3,5-difluorobenzyl)-3-[1-(3-ethynylphenyl)cyclopropylamino]-2-hydroxypropyl]-carbamic acid tert-butyl ester (2.34 g, 5.13 mmol) was treated with 4N HCl in dioxane (15.8 mL, 63.3. mmol). The resulting heterogeneous mixture was treated with methanol (10 mL) whereupon it became homogeneous over 30 min. The volatiles were evaporated in vacuo. Dioxane (20 mL) was added and the mixture was evaporated in vacuo to produce a white solid (2.33 g, 106%).

후처리

  1. customThe volatiles were evaporated in vacuo
  2. additionDioxane (20 mL) was added
  3. customthe mixture was evaporated in vacuo

출처 및 근거

ORD 기록
ord-3966842eb8514e45bf5f87df9672af39
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07727997B2

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