HCID 54440772, 화합물 → HCID 20077534, 화합물

HRID 1655053노트

반응식

HRID 1655053 반응식
C[O:2][C:3]([C:5]1[CH:13]=[C:12]2[C:8]([C:9]([CH2:15][C:16]3[CH:21]=[CH:20][C:19]([O:22][CH2:23][C:24]4[CH:33]=[CH:32][C:31]5[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=5)[N:25]=4)=[CH:18][CH:17]=3)=[CH:10][N:11]2[CH3:14])=[CH:7][CH:6]=1)=[O:4]>[OH-].[Na+].O1CCCC1.CO.O>[CH3:14][N:11]1[C:12]2[C:8](=[CH:7][CH:6]=[C:5]([C:3]([OH:4])=[O:2])[CH:13]=2)[C:9]([CH2:15][C:16]2[CH:17]=[CH:18][C:19]([O:22][CH2:23][C:24]3[CH:33]=[CH:32][C:31]4[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=4)[N:25]=3)=[CH:20][CH:21]=2)=[CH:10]1

참가 물질

6

반응물 1

HCID 54440772HCID 54440772, 화합물

생성물 1

HCID 20077534HCID 20077534, 화합물수율 59.7%

시약·촉매·용매 4

HCID 887Methanol용매HCID 962Water용매HCID 8028Tetrahydrofuran용매HCID 14798Sodium Hydroxide용매

실험 절차

A solution of the methyl ester (Example 10, part ii) (1.73 g) in aqueous sodium hydroxide (2M, 5.9 ml), tetrahydrofuran (20 ml) and methanol (10 ml) was refluxed with stirring overnight. The reaction mixture was cooled, diluted with water until turbid and washed with diethyl ether (2×). The aqueous phase was acidified with acetic acid and the resulting precipitate filtered, washed with water and dried in vacuo at 50° C. to give the product as a white solid (1 g). A small amount was crystallised from tetrahydrofuran/ethanol m.p. 208°-212° C.

후처리

  1. temperatureThe reaction mixture was cooled
  2. washwashed with diethyl ether (2×)
  3. filtrationthe resulting precipitate filtered
  4. washwashed with water
  5. customdried in vacuo at 50° C.

출처 및 근거

ORD 기록
ord-11841f544d40485eaefa555b93fd970f
출처 데이터셋
uspto-grants-1995_04
특허 번호
US05410061

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