Hydrochloric Acid → HCID 12831967、化合物

HRID 1903581ノート

反応式

HRID 1903581 の反応式
Cl.O.[Br:3][C:4]1[CH:5]=[C:6]2[C:11](=[C:12]([Cl:14])[CH:13]=1)[O:10][CH2:9][CH2:8][C:7]2=O>[Zn].C1(C)C=CC=CC=1>[Br:3][C:4]1[CH:5]=[C:6]2[C:11](=[C:12]([Cl:14])[CH:13]=1)[O:10][CH2:9][CH2:8][CH2:7]2

参加物

6

反応物 3

HCID 313Hydrochloric Acid2 回HCID 962Water2 回HCID 128319666-bromo-8-chloro-3,4-dihydro-2H-1-benzopyran-4-one

生成物 1

HCID 12831967HCID 12831967、化合物収率 50.3%

試薬・触媒・溶媒 2

HCID 23994Zinc触媒2 回HCID 1140Toluene溶媒

実験手順

To the amalgam of zinc--prepared from 1280 g (19.7 gram-atoms) of zinc, 128 g (5.4×10-1M) of mercurous chloride, 64 cm3 of concentrated hydrochloric acid and 1900 cm3 of water--are added, in order, 1000 cm3 water, 1500 cm3 of concentrated hydrochloric acid, 3500 cm3 of toluene and 640 g (2.45 M) of 6-bromo-8-chloro-4-chromanone (III2). The mixture is refluxed for 1 hour and, after cooling and decantation, it is extracted with ether and washed in water up to neutrality. 305 g (yield=50%) of expected product are thus isolated. B.p.0.01 =128° C.

後処理

  1. temperatureThe mixture is refluxed for 1 hour
  2. temperatureafter cooling
  3. extractiondecantation, it is extracted with ether
  4. washwashed in water up to neutrality

出典と根拠

ORDレコード
ord-0fe9e13c451e44e1a2d70070aa1b89c3
出典データセット
uspto-grants-1984_03
特許番号
US04436915

反応ノート

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