Hydrazine hydrate (1:1) → HCID 86615670, compound

HRID 507164Notes

Reaction equation

HRID 507164 reaction equation
[F:1][C:2]([F:55])([F:54])[C:3]1[CH:4]=[C:5]([CH:47]=[C:48]([C:50]([F:53])([F:52])[F:51])[CH:49]=1)[CH2:6][N:7]([C@H:26]1[CH2:32][CH2:31][CH2:30][N:29]([CH2:33][CH:34]2[CH2:36][CH2:35]2)[C:28]2[C:37]([CH3:46])=[C:38]([C:42]([F:45])([F:44])[F:43])[C:39]([CH3:41])=[CH:40][C:27]1=2)[C:8]1[N:9]=[N:10][N:11]([CH2:13][CH2:14][N:15]2C(=O)C3C(=CC=CC=3)C2=O)[N:12]=1.O.NN>CO>[NH2:15][CH2:14][CH2:13][N:11]1[N:10]=[N:9][C:8]([N:7]([CH2:6][C:5]2[CH:4]=[C:3]([C:2]([F:1])([F:54])[F:55])[CH:49]=[C:48]([C:50]([F:53])([F:52])[F:51])[CH:47]=2)[C@H:26]2[CH2:32][CH2:31][CH2:30][N:29]([CH2:33][CH:34]3[CH2:35][CH2:36]3)[C:28]3[C:37]([CH3:46])=[C:38]([C:42]([F:44])([F:45])[F:43])[C:39]([CH3:41])=[CH:40][C:27]2=3)=[N:12]1

Participants

4

Procedure

Heat the mixture of (S)-2-(2-{5-[(3,5-Bis-trifluoromethyl-benzyl)-(1-cyclopropylmethyl-7,9-dimethyl-8-trifluoromethyl-2,3,4,5-tetrahydro-1H-benzo[b]azepin-5-yl)-amino]-tetrazol-2-yl}-ethyl)-isoindole-1,3-dione (0.175 g, 0.224 mmol) and hydrazine hydrate (0.1 ml) in methanol (2.0 mL) at 60° C. overnight. Cool down to room temperature. Remove the precipitate by filtration and evaporate the solvent to provide the title compound (0.143 g, 98%). MS (ES+): 650 (M+H).

Workup

  1. temperatureHeat
  2. customRemove the precipitate
  3. filtrationby filtration
  4. customevaporate the solvent

Sources & evidence

ORD record
ord-530fa714b3fe417c853faf37c21dda1f
Source dataset
uspto-grants-2010_08
Patent number
US07786108B2

Reaction notes

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