Hydrochloric Acid → 9-Hydroxy-9H-indeno[1,2-b]pyrazine-2,3(1H,4H)-dione

HRID 129446

반응식

HRID 129446 반응식
[NH:1]1[C:6](=[O:7])[C:5](=[O:8])[NH:4][C:3]2[C:9]3[CH:10]=[CH:11][CH:12]=[CH:13][C:14]=3[C:15](=[O:16])[C:2]1=2.O.[BH4-].[Na+].Cl>C(O)C>[OH:16][CH:15]1[C:2]2[NH:1][C:6](=[O:7])[C:5](=[O:8])[NH:4][C:3]=2[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:14]1=2

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962Water2회HCID 4311764Sodium borohydrideHCID 190359779H-Indeno[1,2-b]pyrazine-2,3,9(1H,4H)-trione

생성물 1

HCID 190359859-Hydroxy-9H-indeno[1,2-b]pyrazine-2,3(1H,4H)-dione수율 91%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a stirred suspension of 9H-indeno[1,2-b]pyrazine-2,3,9(1H,4H)-trione. 1H2O (5.0 g, 21.5 mmol) in 200 ml of ethanol and 30 ml of water was added sodium borohydride (1.76 g, 46.5 mmol) in four portions over 2 hours, then 200 ml of water was added and the mixture was stirred for 18 hours at room temperature. The reaction mixture was acidified with hydrochloric acid (70 ml, 1N) to pH 1.5 and the precipitate was filtered off, washed with water and dried to give 4.59 g (91%) of the title compound. M.p. >300° C. 1H-NMR (DMSO-d6, δ): 5.1 (d, 1H), 5.72 (d, 1H), 7.15 (t, 1H), 7.28 (t, 1H), 7.41 (d, 1H), 7.48 (d, 1H), 12.0 (s, 1H), 12.25 (s, 1H).

후처리

  1. filtrationthe precipitate was filtered off
  2. washwashed with water
  3. customdried

출처 및 근거

ORD 기록
ord-c41c5b63054b47528ee23fd73a0170d4
출처 데이터셋
uspto-grants-1995_11
특허 번호
US05468748

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