Potassium Carbonate → HCID 70543145、化合物

HRID 1156174ノート

反応式

HRID 1156174 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[S:9][C:8]3[CH:10]=[C:11]([CH2:14][C:15]([OH:17])=[O:16])[CH:12]=[CH:13][C:7]=3[C:6]=2[CH:18]=1.C(=O)([O-])[O-].[K+].[K+].Cl.[CH3:26][N:27]([CH2:29][CH2:30]Cl)[CH3:28]>CN(C)C=O>[ClH:1].[CH3:26][N:27]([CH3:28])[CH2:29][CH2:30][O:16][C:15](=[O:17])[CH2:14][C:11]1[CH:12]=[CH:13][C:7]2[C:6]3[CH:18]=[C:2]([Cl:1])[CH:3]=[CH:4][C:5]=3[S:9][C:8]=2[CH:10]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 11636816N,N-Dimethylaminoethyl chloride hydrochlorideHCID 130651048-Chlorodibenzothiophene-3-acetic acid

生成物 1

HCID 70543145HCID 70543145、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 2.76 g. of 8-chlorodibenzothiophene-3-acetic acid, 3.04 g. of potassium carbonate, 1.73 g. of dimethylaminoethyl chloride hydrochloride, and 250 ml. of dimethylformamide was stirred and heated at 120° for 4 hours. The solvent was removed in vacuo on the steam bath, and 75 ml. of water added to the residue. The oil was extracted with ethyl acetate and the crude product precipitated as the hydrochloride by the addition of hydrogen chloride. On crystallization from acetone, 1.5 g. of 8-chlorodibenzothiophene-3-acetic acid 2-dimethylaminoethyl ester hydrochloride, m.p. 179°-181°, was obtained.

後処理

  1. additionA mixture of 2.76 g
  2. temperatureheated at 120° for 4 hours
  3. customThe solvent was removed in vacuo on the steam bath, and 75 ml
  4. additionof water added to the residue
  5. extractionThe oil was extracted with ethyl acetate
  6. customthe crude product precipitated as the hydrochloride by the addition of hydrogen chloride
  7. customOn crystallization from acetone, 1.5 g

出典と根拠

ORDレコード
ord-c88c0a5218804a50aafec4f596fdd1d2
出典データセット
uspto-grants-1982_06
特許番号
US04334078

反応ノート

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