Hydrazine hydrate (1:1) → HCID 178462811、化合物

HRID 1884912ノート

反応式

HRID 1884912 の反応式
[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

参加物

5

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 178462814HCID 178462814、化合物

生成物 1

HCID 178462811HCID 178462811、化合物収率 94%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 887Methanol溶媒

実験手順

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)+.

後処理

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

出典と根拠

ORDレコード
ord-057a31e2ffd44139bfa6ff014fc0f5b6
出典データセット
uspto-grants-2004_07
特許番号
US06767906B2

反応ノート

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