Hydrazine hydrate (1:1) → HCID 178462811, 화합물

HRID 1884912노트

반응식

HRID 1884912 반응식
[CH2:1]([N:3]1[CH:11]=[N:10][C:9]2[C:4]1=[N:5][C:6]([NH:22][C@H:23]1[CH2:28][CH2:27][C@H:26]([OH:29])[CH2:25][CH2:24]1)=[N:7][C:8]=2[NH:12][C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([N+:19]([O-])=O)[CH:14]=1)[CH3:2].O.NN>CO.[Ni]>[NH2:19][C:15]1[CH:14]=[C:13]([NH:12][C:8]2[N:7]=[C:6]([NH:22][C@H:23]3[CH2:24][CH2:25][C@H:26]([OH:29])[CH2:27][CH2:28]3)[N:5]=[C:4]3[C:9]=2[N:10]=[CH:11][N:3]3[CH2:1][CH3:2])[CH:18]=[CH:17][CH:16]=1

참가 물질

5

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 178462814HCID 178462814, 화합물

생성물 1

HCID 178462811HCID 178462811, 화합물수율 94%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 887Methanol용매

실험 절차

A flask is charged with 795 mg (2 mmol) of trans-4-[9-ethyl-6-(3-nitro-phenylamino)-9H-purin-2-yl-amino]-cyclohexanol in 75 ml of methanol and kept under argon. At 40° C. 40 mg of Raney-Nickel is added slowly, followed by addition of 1 ml (31 mmol) of hydrazine monohydrate. After completion the reaction mixture is filtered, the filtrate concentrated and the crude product is taken up into EtOAc (300 ml), extracted with water, dried and evaporated to obtain trans-4-[6-(3-amino-phenylamino)-9-ethyl-9H-purin-2-yl-amino]-cyclohexanol (94% yield); m.p. 149-151° C.; ESI-MS: 368 (M+H)+.

후처리

  1. customAt 40° C
  2. filtrationAfter completion the reaction mixture is filtered
  3. concentrationthe filtrate concentrated
  4. extractionextracted with water
  5. customdried
  6. customevaporated

출처 및 근거

ORD 기록
ord-057a31e2ffd44139bfa6ff014fc0f5b6
출처 데이터셋
uspto-grants-2004_07
특허 번호
US06767906B2

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