Hydrochloric Acid → tert-Butyl propiolate

HRID 349072

反応式

HRID 349072 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.O1CCO[CH2:37][CH2:36]1>CO>[C:6]([C:36]#[CH:37])([O:5][C:1]([CH3:2])([CH3:3])[CH3:4])=[O:33]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 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 360%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

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-cd9b0323cdc74c188f142cd7af870c28
出典データセット
uspto-grants-2007_02
特許番号
US07176242B2

関連ノート

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