Acetone → HCID 86741592、化合物

HRID 652779ノート

反応式

HRID 652779 の反応式
CO[C:3]1[CH:11]=[C:10]([NH2:12])[C:9]([S:13](CC)(=[O:15])=[O:14])=[CH:8][C:4]=1[C:5]([OH:7])=O.C[C:19]([CH3:21])=O.Cl[C:23](OCC(C)C)=[O:24].[CH:30]1([CH2:36][N:37]2[CH2:41][CH2:40][CH:39]([NH2:42])[CH2:38]2)[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31]1>O.C(N(CC)CC)C>[CH:30]1([CH2:36][N:37]2[CH2:41][CH2:40][CH:39]([NH:42][C:5](=[O:7])[C:4]3[CH:8]([O:24][CH3:23])[C:9](=[S:13](=[O:14])=[O:15])[C:10]([NH2:12])=[C:11]([CH2:19][CH3:21])[CH:3]=3)[CH2:38]2)[CH2:31][CH2:32][CH2:33][CH2:34][CH2:35]1

参加物

7

反応物 4

HCID 180AcetoneHCID 62365Isobutyl chloroformateHCID 30182324-Amino-5-(ethylsulphonyl)-o-anisic acidHCID 218906401-(Cyclohexylmethyl)pyrrolidin-3-amine

生成物 1

HCID 86741592HCID 86741592、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 8471Triethylamine溶媒

反応条件

温度
0 °C

実験手順

7.8 g of 2-methoxy-4-amino-5-ethylsulphonyl benzoic acid, 70 ml of acetone, 10 ml of water and 3 g of triethylamine are placed in a 250 ml flask fitted with an agitator, a thermometer and a dropping funnel. The mixture is cooled to 0° C. and 4.1 g of isobutyl chloroformate is poured in drop by drop. It is agitated for 45 minutes at 0° C. and 6 g of 1-cyclohexylmethyl-3-amino-pyrrolidine is dripped in. The reaction is continued for 2 hours at room temperature, 80 ml of water and 5 ml of soda lye are added, then the acetone is evaporated under vacuum. An oil is decanted; it is washed twice with 100 ml of water than dissolved hot in 50 ml ethyl acetate. It is chilled in a refrigerator. The crystals are filtered off, washed with a little ethyl acetate then dried in an oven at 50° C.

後処理

  1. customfitted with an agitator
  2. waitThe reaction is continued for 2 hours at room temperature
  3. customthe acetone is evaporated under vacuum
  4. customAn oil is decanted
  5. washit is washed twice with 100 ml of water
  6. dissolutionthan dissolved hot in 50 ml ethyl acetate
  7. temperatureIt is chilled in a refrigerator
  8. filtrationThe crystals are filtered off
  9. washwashed with a little ethyl acetate
  10. customthen dried in an oven at 50° C.

出典と根拠

ORDレコード
ord-af554a65b7584f12b9b65bc91abfaa7a
出典データセット
uspto-grants-1987_06
特許番号
US04673686

反応ノート

読み込み中…