Propionic Acid → HCID 70613469、化合物

HRID 2083751

反応式

HRID 2083751 の反応式
[Cl:1][C:2]1[CH:15]=[CH:14][C:13]2[O:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]([CH:17]3[CH2:22][CH2:21][N:20]([CH3:23])[CH2:19][CH2:18]3)(O)[C:4]=2[CH:3]=1.S(C1C=CC=CC=1[C:30]([O:32]C(=O)C1C=CC=CC=1S(O)(=O)=O)=[O:31])(O)(=O)=O.[C:49]([OH:53])(=[O:52])[CH2:50][CH3:51].[OH-].[Na+]>O>[C:30]([OH:32])(=[O:31])/[CH:51]=[CH:50]\[C:49]([OH:53])=[O:52].[Cl:1][C:2]1[CH:15]=[CH:14][C:13]2[O:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5](=[C:17]3[CH2:22][CH2:21][N:20]([CH3:23])[CH2:19][CH2:18]3)[C:4]=2[CH:3]=1

参加物

6

反応物 4

HCID 1032Propionic AcidHCID 14798Sodium HydroxideHCID 118096639H-Xanthen-9-ol, 2-chloro-9-(1-methyl-4-piperidinyl)-HCID 13795534Sulphobenzoic anhydride

生成物 1

HCID 70613469HCID 70613469、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

A mixture of 12.5 g. (0.038 m.) of the xanthene-9-ol, 14.0 g. (0.76 m.) of o-sulfobenzoic anhydride and 380 ml. of propionic acid is refluxed for three hours. The reaction mixture is heated in vacuo at 100° C. and the resulting syrup is dissolved in water, made strongly basic with 40% sodium hydroxide solution, extracted with ether, and the dried extract is evaporated. The residual free base is dissolved in ethyl acetate and maleic acid (4.4 g.) is added to yield 4-(2-chloro-9-xanthenylidene)-1-methylpiperidine maleate, m.p. 206°-207° C.

後処理

  1. additionA mixture of 12.5 g
  2. extractionextracted with ether
  3. extractionthe dried extract
  4. customis evaporated
  5. dissolutionThe residual free base is dissolved in ethyl acetate
  6. additionmaleic acid (4.4 g.) is added

出典と根拠

ORDレコード
ord-2c4b050a73984c9c8316ee23d073ec72
出典データセット
uspto-grants-1978_04
特許番号
US04086350

関連ノート

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