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Triethylamine → N-(1-cyclohexylmethyl-2-pyrrolidinyl-methyl)-2,3-dimethoxy-5-sulphamoyl benzamide

HRID 652767
ノート
印刷プレビュー

反応式

HRID 652767 の反応式
[CH3:1][O:2][C:3]1[C:11]([O:12][CH3:13])=[CH:10][C:9]([S:14](=[O:17])(=[O:16])[NH2:15])=[CH:8][C:4]=1[C:5]([OH:7])=O.C(N(CC)CC)C.ClC(OCC)=O.[CH:31]1([CH2:37][N:38]2[CH2:42][CH2:41][CH2:40][CH:39]2[CH2:43][NH2:44])[CH2:36][CH2:35][CH2:34][CH2:33][CH2:32]1>CC(C)=O.O>[CH:31]1([CH2:37][N:38]2[CH2:42][CH2:41][CH2:40][CH:39]2[CH2:43][NH:44][C:5](=[O:7])[C:4]2[CH:8]=[C:9]([S:14](=[O:17])(=[O:16])[NH2:15])[CH:10]=[C:11]([O:12][CH3:13])[C:3]=2[O:2][CH3:1])[CH2:32][CH2:33][CH2:34][CH2:35][CH2:36]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 30176982,3-Dimethoxy-5-sulphamoylbenzoic acidHCID 21268496[1-(Cyclohexylmethyl)pyrrolidin-2-yl]methanamine

生成物 1

HCID 54427560N-(1-cyclohexylmethyl-2-pyrrolidinyl-methyl)-2,3-dimethoxy-5-sulphamoyl benzamide

試薬・触媒・溶媒 2

HCID 180
Acetone
溶媒
HCID 962Water溶媒

実験手順

26.1 g of 2,3-dimethoxy-5-sulphamoyl-benzoic acid (0.10 mole), 40 ml of water, 200 ml of acetone and 10.1 g of triethylamine (0.10 mole) are placed in a 500 ml flask fitted with an agitator, a thermometer and a dropping funnel. The solution is cooled to between 0° and +5° C. and 10.9 g of ethyl chloroformate (0.10 mole) is added drop by drop. It is agitated for 1 hour 30 with the temperature kept at about +5° C., then 19.6 g of 1-cyclohexylmethyl-2-aminomethyl pyrrolidine (0.10 mole) is added drop by drop. A precipitate forms progressively as more and more is added. The reaction medium is then agitated at room temperature, after which it is left to stand. The crystals are filtered, washed three times with water then with 100 ml of 10% ammonia and dried in an oven at 50° C. 50 g is obtained.

後処理

  1. customfitted with an agitator
  2. temperatureThe solution is cooled to between 0° and +5° C.
  3. customkept at about +5° C.
  4. additionA precipitate forms progressively as more and more is added
  5. stirringThe reaction medium is then agitated at room temperature
  6. waitafter which it is left
  7. filtrationThe crystals are filtered
  8. washwashed three times with water
  9. dry with materialwith 100 ml of 10% ammonia and dried in an oven at 50° C
  10. custom50 g is obtained

出典と根拠

ORDレコード
ord-a4222df6281d437182c1142fee59b460
出典データセット
uspto-grants-1987_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04673686

反応ノート

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