Triethylamine → HCID 14459860, 화합물

HRID 1032703노트

반응식

HRID 1032703 반응식
Cl.Cl.[CH3:3][N:4]([CH3:11])[CH:5]1[CH2:10][CH2:9][CH2:8][NH:7][CH2:6]1.[NH:12]1[C:20]2[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=2)[C:14]([C:21](O)=[O:22])=[N:13]1.C(N(CC)CC)C>ClCCl>[CH3:3][N:4]([CH3:11])[CH:5]1[CH2:10][CH2:9][CH2:8][N:7]([C:21]([C:14]2[C:15]3[C:20](=[CH:19][CH:18]=[CH:17][CH:16]=3)[NH:12][N:13]=2)=[O:22])[CH2:6]1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 78250Indazole-3-carboxylic acidHCID 14459855N,N-Dimethylpiperidin-3-amine--hydrogen chloride (1/2)

생성물 1

HCID 14459860HCID 14459860, 화합물수율 12.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Dicyclohexycarbodiimide (1.25 g) was added to a stirred solution of 3-dimethylaminopiperidine dihydrochloride (1 g, 5 mmol), indazole3-carboxylic acid (1.05 g, 6 mmol) and triethylamine (1.25 g) in dichloromethane (25 ml). The mixture was stirred for 48 h, filtered and the filtrate extracted with 1M hydrochloric acid. The acid extracts were combined, washed with a little dichloromethane then basified with ammonia solution and back-extracted into chloroform. The extract was dried and evaporated. The residue was chromotographed on silica using methanol-methyl acetate (1:9) as eluent to give the product which was crystallised from a low volume of ethyl acetate to give the product (0.165 g) mp 141-142° C.

후처리

  1. filtrationfiltered
  2. extractionthe filtrate extracted with 1M hydrochloric acid
  3. washwashed with a little dichloromethane
  4. extractionback-extracted into chloroform
  5. customThe extract was dried
  6. customevaporated
  7. customto give the product which
  8. customwas crystallised from a low volume of ethyl acetate

출처 및 근거

ORD 기록
ord-6d67fd237c5e4ef3abcb4da9c38251ab
출처 데이터셋
uspto-grants-1990_09
특허 번호
US04959375

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