Hydrochloric Acid → 1,3,8-Trihydroxy-6-methyl-9(10H)-anthracenone

HRID 470658

反応式

HRID 470658 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([OH:8])[C:5]2[C:9]([C:11]3[C:16]([OH:17])=[CH:15][C:14]([OH:18])=[CH:13][C:12]=3[C:19](=O)[C:4]=2[CH:3]=1)=[O:10].Cl>C(O)(=O)C>[CH3:1][C:2]1[CH:7]=[C:6]([OH:8])[C:5]2[C:9]([C:11]3[C:16]([OH:17])=[CH:15][C:14]([OH:18])=[CH:13][C:12]=3[CH2:19][C:4]=2[CH:3]=1)=[O:10]

参加物

4

反応物 2

HCID 313Hydrochloric Acid2 回HCID 3220Emodin

生成物 1

HCID 1226351,3,8-Trihydroxy-6-methyl-9(10H)-anthracenone収率 95.4%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A mixture of 20 grams of emodin, 1000 mL of acetic acid, 82.8 grams of stannous chloride was heated to reflux. Hydrochloric acid (60 mL) was added slowly in minutes and continued reflux for 1 hour. Remaining 167 mL of HCl was added slowly at reflux and continued for an additional 1 hour. Orange color mixture was cooled to room temperature and left over night. Product was isolated by filtration and washed with water. Finally the product (emodin anthrone) was dried in vacuo at 60° C. to a constant weight to afford 18.1 grams (Yield: 95%) of an orange powder.

後処理

  1. temperaturewas heated to reflux
  2. temperaturecontinued reflux for 1 hour
  3. additionwas added slowly
  4. temperatureat reflux
  5. waitleft over night
  6. customProduct was isolated by filtration
  7. washwashed with water
  8. dry with materialFinally the product (emodin anthrone) was dried in vacuo at 60° C. to a constant weight

出典と根拠

ORDレコード
ord-6f789f8da53a432bad8ff41fd920e6e6
出典データセット
uspto-grants-2014_01
特許番号
US08629302B2

関連ノート

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