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HCID 13371034, 화합물 → HCID 70410313, 화합물

HRID 1380408
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HRID 1380408 반응식
[CH3:1][O:2][CH2:3][C:4]1[O:8][N:7]=[C:6]([NH2:9])[CH:5]=1.[OH:10][C:11]1[C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=2[S:14](=[O:22])(=[O:21])[N:13]([CH3:23])[C:12]=1[C:24](OC)=[O:25]>C1(C)C(C)=CC=CC=1>[OH:10][C:11]1[C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=2[S:14](=[O:22])(=[O:21])[N:13]([CH3:23])[C:12]=1[C:24]([NH:9][C:6]1[CH:5]=[C:4]([CH2:3][O:2][CH3:1])[O:8][N:7]=1)=[O:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 13371034HCID 13371034, 화합물HCID 54676532methyl 4-hydroxy-2-methyl-2H-1,2-benzothiazine-3-carboxylate 1,1-dioxide

생성물 1

HCID 70410313HCID 70410313, 화합물수율 22.3%

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

A mixture of 0.52 g (4 mmole) of 5-(methoxymethyl)-3-isoxazolamine, 1.08 g (4 mmole) of methyl 4-hydroxy-2-methyl-2H-1,2-benzothiazine-3-carboxylate 1,1-dioxide, and 100 ml of xylene is heated at reflux for six hours in a soxhlet apparatus, the thimble of which contains 20 g of Linde type 4A molecular sieve. The reaction mixture is filtered to clarify it and is allowed to stand at room temperature overnight when the product crystallizes out. The product is filtered, washed with methanol-ether mixture, and then recrystallized from methanol to give 0.326 g of white crystals, mp 218°-223° C. dec.

후처리

  1. temperatureis heated
  2. temperatureat reflux for six hours in a soxhlet apparatus
  3. filtrationThe reaction mixture is filtered
  4. customwhen the product crystallizes out
  5. filtrationThe product is filtered
  6. washwashed with methanol-ether mixture
  7. customrecrystallized from methanol

출처 및 근거

ORD 기록
ord-38491a61eb7a48999c4aa4c65b76a891
출처 데이터셋
uspto-grants-1986_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04581458

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