Trichloroacetic Acid → 2-[2-(bis-(2-chloroethyl)-amino)-2-oxo-tetrahydro-2H-1,3,2-oxazaphosphorin-4-yl-thio]-ethanesulphonic acid ammonium salt

HRID 1731964

반응식

HRID 1731964 반응식
[CH2:1]1[CH:7](O)[NH:6][P:4]([N:9]([CH2:13][CH2:14][Cl:15])[CH2:10][CH2:11][Cl:12])(=[O:5])[O:3][CH2:2]1.[NH4+].[SH:17][CH2:18][CH2:19][S:20]([O-:23])(=[O:22])=[O:21].ClC(Cl)(Cl)C(O)=O>O>[NH4+:6].[Cl:12][CH2:11][CH2:10][N:9]([CH2:13][CH2:14][Cl:15])[P:4]1(=[O:5])[NH:6][CH:7]([S:17][CH2:18][CH2:19][S:20]([O-:23])(=[O:22])=[O:21])[CH2:1][CH2:2][O:3]1

참가 물질

5

반응물 3

HCID 6421Trichloroacetic AcidHCID 997354-HydroxycyclophosphamideHCID 23049872Ammonium 2-mercaptoethanesulphonate

생성물 1

HCID 1101861772-[2-(bis-(2-chloroethyl)-amino)-2-oxo-tetrahydro-2H-1,3,2-oxazaphosphorin-4-yl-thio]-ethanesulphonic acid ammonium salt

시약·촉매·용매 1

HCID 962Water용매

실험 절차

2.8 g (10 mmol) of 4-hydroxycyclophosphamide and 1.6 g (10 mmol) of ammonium-2-mercaptoethanesulphonate were dissolved together with a catalytic quantity of trichloroacetic acid in 50 ml of water and were left to stand in a refrigerator for 3 days at 0° C. The water was then distilled off under high vacuum, the residue was taken up twice in acetone and concentrated under vacuum. Recrystallisation from acetone/ether.

후처리

  1. waitwere left
  2. distillationThe water was then distilled off under high vacuum
  3. concentrationconcentrated under vacuum
  4. customRecrystallisation from acetone/ether

출처 및 근거

ORD 기록
ord-e302beff77d74df68565ed600e715631
출처 데이터셋
uspto-grants-1986_11
특허 번호
US04623742

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