Water → D-Tartrate

HRID 379311노트

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HRID 379311 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH2:7][C:8]12[C:16](=[O:17])[N:15]([CH2:18][C:19]([F:22])([F:21])[F:20])[C:14](=[O:23])[N:9]1[CH2:10][CH2:11][NH:12][CH2:13]2.O.[C:25]([OH:34])(=[O:33])[C@H:26]([C@@H:28]([C:30]([OH:32])=[O:31])[OH:29])[OH:27]>CC(C)=O>[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH2:7][C@:8]12[C:16](=[O:17])[N:15]([CH2:18][C:19]([F:21])([F:22])[F:20])[C:14](=[O:23])[N:9]1[CH2:10][CH2:11][NH:12][CH2:13]2.[C:30]([C@H:28]([C@@H:26]([C:25]([O-:34])=[O:33])[OH:27])[OH:29])([O-:32])=[O:31]

참가 물질

6

반응물 3

HCID 962WaterHCID 439655D-Tartaric acidHCID 113364048a-Pyridin-2-ylmethyl-2-(2,2,2-trifluoro-ethyl)-tetrahydro-imidazo[1,5-a]pyrazine-1,3-dione

생성물 2

HCID 5460284D-Tartrate수율 73%HCID 11537198HCID 11537198, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

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온도
56 °C

실험 절차

To a solution of 8a-pyridin-2-ylmethyl-2-(2,2,2-trifluoro-ethyl)-tetrahydro-imidazo[1,5-a]pyrazine-1,3-dione (prepared according to the method described in Step 6, 106 g, 0.325 mol) in acetone (2120 mL) and water (212 mL) was added D-tartaric acid (48.46 g, 0.325 mol). White precipitate formed and it was granulated for 3 hours. The solids were collected by suction filtration and washed with acetone. The solvent damp solids were placed in acetone (1000 mL) and stirred at 56° C. overnight. The solids were collected by suction filtration the next morning and dried to give 56 g of the chiral title compound as the D-tartrate salt (73% yield of theory). Chiral HPLC showed an optical purity of 98:2.

후처리

  1. customWhite precipitate
  2. customformed
  3. filtrationThe solids were collected by suction filtration
  4. washwashed with acetone
  5. filtrationThe solids were collected by suction filtration the next morning
  6. customdried

출처 및 근거

ORD 기록
ord-7f96caa8f9cc432f962c3bc852bb4e8a
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06297380B1

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