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Acetone → 4-[[[4-(hexahydro-1H-azepin-1-yl)-phenyl]-sulphonyl]-amino]-3-hydroxy butanoic acid

HRID 1590589

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HRID 1590589 반응식

[N:1]1([C:8]2[CH:13]=[CH:12][C:11]([S:14](Cl)(=[O:16])=[O:15])=[CH:10][CH:9]=2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.CC(C)=O.[OH:22][CH:23]([CH2:28][NH2:29])[CH2:24][C:25]([OH:27])=[O:26].N12CCN(CC1)CC2>O>[N:1]1([C:8]2[CH:13]=[CH:12][C:11]([S:14]([NH:29][CH2:28][CH:23]([OH:22])[CH2:24][C:25]([OH:27])=[O:26])(=[O:16])=[O:15])=[CH:10][CH:9]=2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

참가 물질 반응 조건 실험 절차 후처리 출처 및 근거 반응 노트

참가 물질

6

반응물 4

HCID 180Acetone

HCID 21494-Amino-3-hydroxybutanoic acid

HCID 10355958(4-Hexahydro-azepin-1-yl-benzenesulphonyl) chloride

생성물 1

HCID 541188884-[[[4-(hexahydro-1H-azepin-1-yl)-phenyl]-sulphonyl]-amino]-3-hydroxy butanoic acid수율 150.4%

시약·촉매·용매 1

HCID 962

Water

용매

반응 조건

온도: 0 °C

실험 절차

4.1 g of (4-hexahydro-azepin-1-yl-benzenesulphonyl) chloride then 12 cm3 of acetone are added to a solution of 1.4 g of 3-hydroxy-4-amino butanoic acid and 3.36 g of 1,4-diazabicyclo [2.2.2]octane (DABCO) in 18 cm3 of water. Agitation is carried out for 6 hours at ambient temperature, the acetone is evaporated off, the residue is cooled down to 0° C. and 7.5 cm3 of 2N hydrochloric acid is added. Extraction is carried out with chloroform, the extracts are dried and evaporated to dryness. 6.3 g of desired product is obtained, used as it is for the following stage.

후처리

customthe acetone is evaporated off
addition7.5 cm3 of 2N hydrochloric acid is added
extractionExtraction
customthe extracts are dried
customevaporated to dryness

출처 및 근거

ORD 기록: ord-903cc4cb070b497ea3faf895e944aac8
출처 데이터셋: uspto-grants-1993_04
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US05204341

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