Water → 1-(3,5-Dichloro-pyridin-4-ylmethyl)-6-difluoromethoxy-4-morpholin-4-yl-phthalazine

HRID 2268902Notes

Reaction equation

Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([O:12][CH:13]([F:15])[F:14])[CH:10]=2)[C:5]([CH2:16][C:17]2[C:22]([Cl:23])=[CH:21][N:20]=[CH:19][C:18]=2[Cl:24])=[N:4][N:3]=1.[OH2:25]>N1CCOCC1>[Cl:23][C:22]1[CH:21]=[N:20][CH:19]=[C:18]([Cl:24])[C:17]=1[CH2:16][C:5]1[C:6]2[C:11](=[CH:10][C:9]([O:12][CH:13]([F:14])[F:15])=[CH:8][CH:7]=2)[C:2]([N:20]2[CH2:21][CH2:22][O:25][CH2:18][CH2:19]2)=[N:3][N:4]=1

Participants

Conditions

Temperature: 100 °C

Procedure

A suspension under N2 of 4-chloro-1-(3,5-dichloro-pyridin-4-ylmethyl)-6-difluoromethoxy-phthalazine (5.5 g, 14.1 mmoles), prepared as described in example 99, in morpholine (11 ml) was heated at 100° C. for 1 hour, then cooled and poured into water (150 ml). A solid formed and was stirred for 15 minutes, then filtered, washed with water, dried over P2O5 at 50° C. under high vacuum. There were obtained 6 g of the title compound (yield: 96%). m.p.: 128.6-130.6° C.

Workup

temperaturecooled
customA solid formed
filtrationfiltered
washwashed with water
dry with materialdried over P2O5 at 50° C. under high vacuum

Sources & evidence

ORD record: ord-06d7ece2d3684650ad22bbf53391ca83
Source dataset: uspto-grants-2001_12
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US06329370B1

Reaction notes

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