Hydrochloric Acid → tert-Butyl propiolate

HRID 14282

反応式

HRID 14282 の反応式
[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]

参加物

5

反応物 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

生成物 1

HCID 543038tert-Butyl propiolate収率 106%

実験手順

[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%).

後処理

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

出典と根拠

ORDレコード
ord-3966842eb8514e45bf5f87df9672af39
出典データセット
uspto-grants-2010_06
特許番号
US07727997B2

関連ノート

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